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GERSTEL Solutions No. 7 (pdf; 1,86 MB)

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<strong>GERSTEL</strong> MAESTRO Software<br />

Application<br />

Beer flavor analysis<br />

with a twist<br />

Virtuosity<br />

Defined<br />

Report<br />

Wine flavor from<br />

trash cans<br />

Application<br />

Hot in pursuit of<br />

forgers<br />

A passion for performance<br />

Get Gerstelized!


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Editorial<br />

A passion for performance<br />

In this issue<br />

Editorial<br />

<strong>GERSTEL</strong>: 40 Years<br />

Analytical <strong>Solutions</strong> -<br />

A passion for performance 2<br />

Portrait<br />

Asahi: Improving sales<br />

by focusing on quality<br />

and consistency 3<br />

Get Gerstelized!<br />

<strong>GERSTEL</strong> ® is among the leading providers of customer<br />

focused solutions for sample preparation and sample<br />

introduction in chromatography. The company is the<br />

largest partner of Agilent Technologies world-wide for<br />

customer focused analytical solutions. <strong>GERSTEL</strong> was<br />

founded 40 years ago.<br />

Application<br />

Extraction technique:<br />

Beer flavor analysis with a twist 4<br />

Food safety: Fast and<br />

reliable answers regarding<br />

aflatoxins in foods 18<br />

Forensics: Hot in pursuit<br />

of forgers 22<br />

Report<br />

Cover story<br />

<strong>GERSTEL</strong> MAESTRO<br />

Software:<br />

step-by-step<br />

8<br />

Generating<br />

MAESTRO sequences:<br />

Easier than ever<br />

11<br />

Wine analysis:<br />

Flavor from trash cans 12<br />

Distributor<br />

Tegent Technology Ltd.:<br />

<strong>GERSTEL</strong> Distributor for China 15<br />

Innovation<br />

Product highlights at PittCon 2007:<br />

– Automated TubeEXchance ATEX<br />

– Automated SPE<br />

– GC PrepStation<br />

– Automated Dynamic Headspace 16<br />

News<br />

<strong>GERSTEL</strong> expands to<br />

accommodate steady growth 24<br />

As a family business, <strong>GERSTEL</strong> has always<br />

enjoyed freedom from short- or<br />

medium-term interests of investors,<br />

allowing us to pursue promising long-term<br />

strategies and projects. The <strong>GERSTEL</strong> tradition<br />

is to supply a steady stream of innovative<br />

solutions for chromatography sample<br />

handling and sample introduction,<br />

providing increased performance and improved<br />

system ruggedness. “Our philosophy<br />

is to exceed our customers’ expectations”,<br />

says Eberhard G. Gerstel, President<br />

and co-owner of the company. <strong>GERSTEL</strong><br />

has been in the fortunate position to have<br />

sufficient resources to keep and extend our<br />

strong position as a global provider of GC/<br />

MS solutions while adding LC and LC/MS<br />

solutions to our product offering over the<br />

past years. Since 1998, <strong>GERSTEL</strong> has had<br />

double digit annual growth; our organization<br />

has grown by more than 100 % over<br />

the past 5 years. <strong>GERSTEL</strong>, Inc., based in<br />

Baltimore, MD and <strong>GERSTEL</strong> KK, based in<br />

Tokyo, have both contributed strongly, expanding<br />

their service and support departments<br />

and adding further staff to meet increased<br />

demand.<br />

A series of products and solutions, including<br />

most recently Automated SPE and<br />

automated Dynamic Headspace (DHS), have<br />

been developed around the <strong>GERSTEL</strong> MultiPurpose<br />

Sampler (MPS). The MPS is an<br />

integrated autosampler and liquid handling<br />

robot. This year at PittCon, <strong>GERSTEL</strong><br />

showed the new DHS system and the<br />

unique automated SPE system based<br />

on standard cartridges.<br />

Accelerating Performance<br />

The <strong>GERSTEL</strong> SPE can<br />

significantly increase productivity<br />

and throughput<br />

of GC/MS and LC/MS labs,<br />

improving Return on Investment<br />

(ROI) for the instrumentation.<br />

Additional benefits are improved<br />

precision and significantly reduced<br />

solvent consumption with associated savings<br />

and improvements of the laboratory<br />

environment. “Our integrated solutions<br />

and integrated software help control every<br />

step of the process, from automated Sample<br />

Prep through Sample Introduction to control<br />

of the entire LC/MS or GC/MS system.<br />

Just one method and one sequence table<br />

controls the entire process providing simple<br />

and efficient operation with less risk of<br />

error“, says Eberhard G. Gerstel.<br />

<strong>GERSTEL</strong> management is in a mood to celebrate. In 2007,<br />

the company is celebrating its 40th anniversary and the<br />

relocation to new larger headquarters. Pictured from left:<br />

Ralf Bremer, Holger Gerstel, Eberhard G. Gerstel.<br />

<strong>GERSTEL</strong> MPS<br />

with SPE option<br />

2<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Portrait<br />

In 2005, world-wide production of beer amounted to<br />

a volume of around 160 billion liters – or 1.6 billion<br />

hectoliters in brewery-lingo; more than half of this sea<br />

of beer was produced by the ten largest international<br />

brewing conglomerates.<br />

Breweries up their R & D investments<br />

Improving sales by focusing<br />

on quality and consistency<br />

In first position, the Belgian InBev group<br />

produced around 20 billion liters of beer,<br />

almost 13 % of world-wide production.<br />

In second place was SABMiller of the UK<br />

with 17.6 billion liters, narrowly relegating<br />

the US-based brewing giant Anheuser-<br />

Busch (17.4 billion liters/year) to third position.<br />

In 13th position we find Asahi, Japan’s<br />

largest and internationally most successful<br />

brewery.<br />

Asahi was founded in 1887, launching<br />

their first lager beer five years later. In 2005,<br />

Asahi produced around 2.5 billion liters,<br />

equal to 1.5 % of world-wide production.<br />

The trend is clear: further growth!<br />

Research Pays Off<br />

Asahi’s consistent success and solid growth<br />

over many decades is attributed in large<br />

measure to the company’s constant commitment<br />

to research and development<br />

(R&D), which is always striving to produce<br />

the best possible product. The Asahi<br />

R&D Department has around 300 employees,<br />

a relatively large number. The picture<br />

that has emerged is, that in order to gain<br />

ground and stay among the leaders in international<br />

beer markets, breweries must be in<br />

a position to develop products that are attractive<br />

to a large number of different consumer<br />

markets, they must hit the right taste<br />

for these budding markets, and last but not<br />

least, deliver consistent quality.<br />

Analysis Techniques<br />

In the Asahi breweries and in their R&D facilities,<br />

even though a wide range of analytical<br />

techniques are used, chromatography is<br />

the technique most commonly used.<br />

GC and LC systems help control all<br />

stages of production of the many Asahi beverages,<br />

ensuring product quality and consistency.<br />

These techniques are used for development<br />

purposes as well.<br />

Chromatography is used “first when we<br />

develop the products, for example, analyzing<br />

hop flavors; secondly when we work to improve<br />

the quality of existing products; and<br />

thirdly, in our QC and food safety controls,<br />

for example, when we work to eliminate offodors<br />

or variations in product taste or try to<br />

identify what causes these things”, says Mr.<br />

Toru Kishimoto of the Asahi Brewing Research<br />

and Development Laboratory.<br />

Choosing the Right Sample<br />

Preparation Technique<br />

Extraction of target compounds from<br />

complicated beer or wort matrices is often<br />

a challenge. Conventional sample preparation<br />

techniques often are not up to the<br />

task, according to Mr. Kishimoto: “They re-<br />

Mr. Toru Kishimoto talking to Mr.<br />

Hirooki Kanda. Mr. Kanda is Managing<br />

Director of <strong>GERSTEL</strong> K.K., a <strong>GERSTEL</strong>subsidiary<br />

based in Tokyo, Japan.<br />

quire large volumes of solvent, lots of time,<br />

do not provide sufficient recovery or detection<br />

limits - and often they cannot be efficiently<br />

automated”.<br />

Consequently, Asahi has replaced many<br />

conventional sample preparation methods<br />

with Solid Phase Micro Extraction (SPME)<br />

and Stir Bar Sorptive Extraction (SBSE) using<br />

the <strong>GERSTEL</strong> Twister®. Toru Kishimoto:<br />

„These techniques are easy to perform.<br />

They require no solvent, provide low detection<br />

limits, they are fast so they ensure good<br />

sample throughput and are easily automated“.<br />

SBSE is used by Asahi for the determination<br />

of hop flavor compounds as well as<br />

trans-2-nonenal, fatty acids or off-odors.<br />

Asahi currently has a range of <strong>GERSTEL</strong><br />

solutions in their laboratories: MultiPurpose<br />

Sampler (MPS)-GC/MS systems are<br />

used for automated SPME and SBSE analysis.<br />

Thermal Desorption (TDS)-GC/MS systems<br />

are used for automated thermal desorption<br />

of Tenax-filled desorption tubes,<br />

MPS/GC-GC/MS systems are used for<br />

Multi-Dimensional GC analysis and the<br />

<strong>GERSTEL</strong> Preparative Fraction Collector<br />

(PFC) is used for preparative GC. Finally,<br />

GC/MS systems fitted with <strong>GERSTEL</strong> Olfactory<br />

Detector Ports (ODP) provide simultaneous<br />

olfactory and mass spectrometric<br />

detection, using an integrated voice<br />

recognition software package to provide a<br />

detailed “olfactogram” that includes odor<br />

intensity, retention time and voice comments<br />

for compounds as they elute.<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

3


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

Foto: wikipedia<br />

Extraction technique comparison<br />

Beer flavor<br />

analysis with<br />

a twist<br />

Hops contain terpenoids that help<br />

give beer its slightly bitter taste and,<br />

if properly combined and controlled,<br />

a fine flavor. Since variations in terpenoid<br />

concentrations occur during the beer<br />

brewing process, careful monitoring and<br />

adjustment is required in order to achieve<br />

consistent quality. The Asahi Breweries<br />

has succeeded in determining the<br />

concentrations of a long list of relevant<br />

flavor compounds in just one analysis.<br />

To achieve this, Asahi uses Stir Bar<br />

Sorptive Extraction (SBSE).<br />

Beer is one of the oldest and most<br />

widely enjoyed beverages in the<br />

world. Traditionally, beer is based<br />

on four ingredients: Water, barley,<br />

yeast and hops. The barley is allowed to germinate<br />

and is then malted, that is, dried at<br />

elevated temperatures; water is added, and<br />

the malt boiled to form the wort. Hops are<br />

added as the wort boils. After filtering, yeast<br />

is added and the fermentation process puts<br />

its finishing touches to the product. The<br />

temperature used during the malting process<br />

as well as the hops, or rather the terpenoids<br />

they contain, are some of the key factors<br />

in forming the distinct taste of the brew.<br />

Hops and malt additionally serve as natural<br />

preservatives. During the various stages<br />

of the brewing process, variations in terpenoid<br />

concentrations can occur. Careful<br />

monitoring and adjustment is required in<br />

order to achieve consistent quality.<br />

The Asahi Breweries are able to determine<br />

the concentrations of a long list of terpenoids<br />

in modestly sized samples of beers<br />

at all stages of production. This requires<br />

a sensitive technique, especially when analyzing<br />

beer with mild hop flavor, which<br />

is typically preferred in Japan. Asahi relies<br />

on GC/MS in combination with Stir<br />

Bar Sorptive Extraction<br />

(SBSE) using the<br />

<strong>GERSTEL</strong> Twister®. Mr.<br />

Toru Kishimoto and his colleagues<br />

from the Asahi Research<br />

and Development Centre have reported<br />

their findings regarding the advantages of<br />

the Twister technology in comparison with<br />

other techniques, in the Journal of Agricultural<br />

and Food Chemistry [2005; 53(12);<br />

4701-4707].<br />

Conventional techniques are<br />

not always up to the task<br />

While there is general agreement that hop<br />

flavor compounds should be determined<br />

using GC/MS, opinions vary when it comes<br />

to choosing the best extraction technique.<br />

Different laboratories have chosen a wide<br />

variety of techniques to extract and concentrate<br />

hop flavor compounds from beer<br />

in its various stages of production:<br />

Lam et al. [1] let two liters of beer run<br />

through a silica gel column to separate<br />

and determine linaloole, geraniole and -<br />

citronellole that add citrus and floral flavor<br />

notes. Steinhaus and Schieberle [2] extracted<br />

flavor compounds directly from<br />

hops and identified linaloole and myrce-<br />

ne as potential flavour<br />

compounds.<br />

De Keukeleire et al.<br />

[3] extracted a variety of<br />

hops using Supercritical Fluid<br />

Extraction, based on CO 2<br />

, enabling<br />

them to identify myrcene, -Caryophyllene,<br />

-humulene and -farnesene.<br />

In addition to the above, Irwin [4] and<br />

Goiris et al. [5] used a silica gel column<br />

to separate flavor compounds found in<br />

Hersbrucker Beer; demonstrating clearly<br />

that the oxygenated sesquiterpene fraction<br />

contributes to the “hoppy” character of the<br />

beer. This group includes eudesmole, humulene<br />

epoxide and humulenole II among<br />

others. Lermusieau et al. [6] used an XAD<br />

2 resin column to determine that linaloole<br />

and -Damascenone are active flavor<br />

compounds.<br />

Though all the above approaches provide<br />

meaningful results, they still leave a lot<br />

to be desired according to Toru Kishimoto<br />

and his colleagues.: „These techniques require<br />

raw hops and large volumes of sample<br />

in order to extract the active flavor<br />

compounds in sufficient amounts. Furthermore,<br />

these techniques work mainly<br />

for beers that have a strong hop flavor”.<br />

4<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

In order to accurately determine the terpenoid<br />

profile of Japanese beers, that typically<br />

have less intense hop flavor, a more sensitive<br />

analysis technique is needed. According<br />

to the Asahi scientists, conventional extraction<br />

techniques have proven quite complex<br />

and labor intensive and are therefore<br />

not well suited for routine analysis involving<br />

large numbers of samples. One promising<br />

alternative is already used by Asahi to<br />

establish terpenoid profiles: Stir Bar Sorptive<br />

Extraction (SBSE). This technique has<br />

previously proven its worth for the determination<br />

of trace concentrations of VOCs<br />

in beer [7,8].<br />

In practice, SBSE is performed using the<br />

<strong>GERSTEL</strong> Twister, a magnetic stir bar with<br />

a layer of between 24 and 126 μL PDMS<br />

sorbent depending on the type. “The technique<br />

is really easy to handle, up to 1000<br />

times more sensitive than SPME and readily<br />

automated”, Toru Kishimoto and his colleagues<br />

stated.<br />

SBSE compared with<br />

Conventional extraction<br />

In order to determine whether SBSE was<br />

up to the task, the Asahi scientists compared<br />

results from SBSE and a widely used<br />

methylene chloride based liquid/liquid extraction.<br />

Samples used for the comparison<br />

were two commercially available Japanese<br />

beers, one with intense hop flavor, and one<br />

with mild hop flavor. The analysis was performed<br />

using GC/MS; compounds identified<br />

were quantified using the response factor<br />

for -damascenone, added as an internal<br />

standard.<br />

Results: Using conventional methylene<br />

chloride extraction, only three compounds<br />

SBSE is performed using the patented Twister ® .<br />

The Twister is a magnetic stir bar, coated with<br />

glass and surrounded by a PDMS phase of<br />

up to 126 μL. The Twister is immersed into an<br />

aqueous or other liquid sample, in this case<br />

into the beer or wort sample, from which it efficiently<br />

extracts especially the hydrophobic<br />

analytes while stirring.<br />

The efficiency of SBSE for a given compound<br />

correlates well with the partition coefficient<br />

for that compound between polydimethylsiloxane<br />

(PDMS) and water, which in turn correlates<br />

well with its Octanol/Water partition<br />

coefficient K O/W<br />

. K O/W<br />

is a physical parameter<br />

used to describe the hydrophilic or hydrophobic<br />

properties of a chemical compound including<br />

its tendency to accumulate in fat tissue<br />

[10]. The logarithm of the PDMS/water partition<br />

coefficient is almost equal to the logarithm<br />

of the octanol/water partition coefficient<br />

(Log K O/W<br />

), that can be found in standard tables.<br />

A large Log K O/W<br />

value signifies a high<br />

Background on<br />

Stir Bar Sorptive Extraction<br />

degree of hydrophobicity, indicating that the<br />

analyte is highly soluble in PDMS and can be<br />

extracted with good recovery by the Twister ® .<br />

„The PDMS/water phase system reaches<br />

equilibrium faster at higher temperatures“,<br />

Toru Kishimoto and his colleagues report in<br />

the Journal of Agricultural and Food Chemistry.<br />

They chose a temperature of 40 °C, extracting<br />

the sample over two hours; the Log<br />

K O/W<br />

values of the terpenoids ranged from 3.4<br />

to 7.1 and -damascenone was used as internal<br />

standard since its Log K O/W<br />

value of 4.4 was<br />

well within this range. Further, a strong correlation<br />

was observed between the response<br />

factors of -damascenone and all other terpenoids.<br />

The Twisters were subsequently automatically<br />

desorbed using an MPS fitted with<br />

Twister Option in combination with a Thermal<br />

Desorption Unit (TDU). GC/MS was performed<br />

using a GC 6890/MSD 5973N system from<br />

Agilent Technologies.<br />

were identified: Linaloole, geraniole und -<br />

eudesmole. The limited extraction efficiency<br />

was attributed to interference from matrix<br />

components such as proteins, amino<br />

acids and polyphenols.<br />

On the other hand, using SBSE, Kishimoto<br />

and his colleagues were able to identify<br />

a large number of other terpenoids,<br />

among them -eudesmole, humulene, humuleneepoxide<br />

I, -farnesene, caryophyllene<br />

and geraniole. “The results were clear:<br />

The SBSE method enables us to easily determine<br />

a number of compounds that we<br />

were not able to find using the conventional<br />

extraction method.”<br />

Tracking terpenoid levels<br />

throughout the brewing<br />

process<br />

The simplicity of the SBSE method and<br />

the fact that it requires only a small sample<br />

size and very little sample preparation, allowed<br />

the Asahi scientists to monitor both<br />

the presence and the changes in concentrations<br />

of terpenoids during the wort boiling<br />

process. Hops normally contain high<br />

levels of caryophyllene, humulene and -<br />

Farnesene; however, during the wort boiling<br />

process, only small concentrations are<br />

Toru Kishimoto, Laboratory Manager<br />

at Asahi R&D Centre, discusses<br />

results from hop flavor analysis<br />

performed using the <strong>GERSTEL</strong><br />

Twister with a co-worker.<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

5


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

Samples are being extracted by Twister stir bars<br />

prior to GC/MS analysis at the Asahi R&D Centre.<br />

MPS-GC/MS system used by Asahi for the analysis of terpenoids in hops.<br />

found. Kishimoto and his colleagues attribute<br />

this to the poor solubility of terpenoids<br />

in wort. -citronellole was not detected<br />

in wort samples at all. It is formed from<br />

geraniole, but not until the fermentation<br />

step of the brewing process. It was observed<br />

Total Ion Chromatogram of Japanese Beer<br />

that the reduction in terpenoid concentrations<br />

follows two different patterns.<br />

The first pattern was observed for<br />

myrcene and linaloole, whose concentrations<br />

decreased rapidly during the wort<br />

boiling process. The rapid decline is mainly<br />

attributed to the relatively low boiling<br />

points of these compounds (myrcene 167 °C,<br />

linaloole 194 °C). For comparison, humulene<br />

and farnesene have boiling points of<br />

266 °C and 260 °C respectively. Conclusion:<br />

„The hops should not be added to<br />

the wort until the very end of, or even until<br />

after the wort boiling process” according<br />

to Kishimoto et al.<br />

The second pattern they observed was<br />

seen for higher boiling compounds, for example,<br />

-eudesmole, humulene, humuleneepoxide<br />

I, -farnesene, caryophyllene<br />

and geraniole: The concentrations of these<br />

compounds decreased slowly and linearly<br />

as a function of time over the course of<br />

the wort boiling process. „Both observations<br />

support our contention, that the degree<br />

to which a beer has a hop-based character<br />

is directly dependent on the point in<br />

time at which the hops were added to the<br />

brew“, the scientists said.<br />

Comparison between chromatograms from beer samples using standard liquid extraction (top) and Stir Bar<br />

Sorptive Extraction (SBSE) with the <strong>GERSTEL</strong> Twister (bottom). The result is extremely clear, according to<br />

Toru Kishimoto: ”SBSE is an extremely sensitive analysis technique, providing us with very low detection<br />

limits. It operates without the use of solvents, is easy to handle, produces first rate results, and enables the<br />

determination of a large number of compounds in one analytical run.“<br />

Terpenoids<br />

Terpenoids, sometimes referred to as<br />

isoprenoids, are extensively used for<br />

their aromatic qualities. Terpenoid profiles<br />

form important characteristics,<br />

even enabling the identification of<br />

plants by their profile. More than 30,000<br />

terpenoids are known, 8000 of which also<br />

belong to the chemical compound<br />

group terpenes. Source: wikipedia<br />

6<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

Materials, Reagents and Methods<br />

Reagents<br />

Linaloole, geraniole, myrcene, caryophyllene,<br />

-humolene, -damascenone and -damascone<br />

from Fluka (Steinhaus, Switzerland); -<br />

citronelle and cis-3-Heptene-1-ol from Sigma-Aldrich<br />

(St. Louis, MO) and from Avocado<br />

Research Chemicals Ltd. (Lancashire, U.K.).<br />

Eudesmol, -farnesene and synthetic humulene<br />

epoxide from Wako (Osaka, Japan). All<br />

reagents were Analytical Grade.<br />

SBSE Method: CV and<br />

Detection Limits<br />

CV (%)<br />

Detection<br />

Limit (ppb)<br />

(S/N=3)<br />

Linalool 4.3 0.049<br />

Geraniol 5.7 0.099<br />

Citronellol 6.8 0.278<br />

Myrcene 7.4 0.001<br />

Caryophyllene 8.2 0.031<br />

a-Humulene 4.2 0.035<br />

Humulene epoxide1 2.5 0.044<br />

Eudesmol 5.5 0.013<br />

b-Farnesene 6.7 0.023<br />

b-Damascenone 2.0 0.019<br />

Liquid extraction using methylene chloride<br />

A 350 mL beer sample was taken and 5 μL of a<br />

cis-3-heptene-1-ol solution added as internal<br />

standard. Liquid extraction was performed<br />

by adding 150 mL dichloromethane and allowing<br />

the extraction to proceed for 3 hours.<br />

After separating the dichloromethane, it was<br />

dried with anhydrous sodium sulphate for 30<br />

minutes and concentrated to approximately<br />

1 mL in a rotary evaporator at 40 °C under<br />

vacuum (750 hPa).<br />

GC/MS method used for the liquid extract<br />

An Agilent ® Technologies GC 6890 coupled<br />

with a 5973 N MSD quadropole mass spectrometer<br />

was used for the analysis. The column<br />

used was a DB-WAX, 60 m length x 0.25<br />

mm i.d., 0.25 μm film thickness from Agilent<br />

Technologies. GC: 1 μL extract was introduced<br />

to the GC in splitless, pressure pulsed<br />

mode. Inlet temperature: 250 °C. Helium was<br />

used as carrier gas at constant flow of 1 mL/<br />

min. Oven temperature program: Initial temperature<br />

40 °C , held for 5 min. Ramped at<br />

3 °C /min to 240 °C and held for 20 min. MSD:<br />

Scan range: 30 – 359 (m/z); EI mode, ionization<br />

energy: 70 eV. All compounds were identified<br />

on the basis of their mass spectra as<br />

well as on the retention time. Standard mixtures<br />

were used in order to compare spectra<br />

and retention times with those of authenticated<br />

compounds.<br />

Sample Preparation for Stir Bar Sorptive<br />

Extraction (SBSE) using the <strong>GERSTEL</strong><br />

Twister ®<br />

The <strong>GERSTEL</strong> Twisters used were 20 mm<br />

long, coated with 47 μL Polydimethylsiloxane<br />

(PDMS). Prior to their use, the Twisters were<br />

conditioned under a flow of Helium for one<br />

hour at 300 °C. 0.1 ppb -damascenone was<br />

added to the sample (beer or wort) as internal<br />

standard. A 30 mL sample was diluted fourfold<br />

with distilled water and the Twister added.<br />

The vial was sealed and was stirred using<br />

the Twister for 2 hours at 40 °C. Following<br />

the extraction step, the Twister was removed<br />

from the sample, rinsed with distilled water<br />

and dabbed dry on lint-free paper cloth. The<br />

Twisters were desorbed in the Thermal Desorption<br />

Unit (TDU), mounted on the <strong>GERSTEL</strong><br />

CIS inlet. Using the <strong>GERSTEL</strong> MultiPurpose<br />

Sampler (MPS) up to 196 Twisters can be processed<br />

in one automated sequence. Prior to<br />

GC/MS determination, analytes were concentrated<br />

in the Cooled Injection System (CIS)<br />

and subsequently transferred to the column<br />

using a CIS temperature program.<br />

Analyte quantitation was performed using<br />

the following m/z target ions: 69 (geraniole),<br />

80 (-humulene), 85 (humulenole), 93 (linalo-<br />

Literature<br />

[1] Lam, K. C.; Foster, R. T.; Deinzer, M. L. Aging of hops<br />

and their contribution to beer flavor. J. Agric. Food<br />

Chem. 19<strong>86</strong>, 34, 763-779.<br />

[2] Steinhaus, M.; Schieberle, P. Comparison of the most<br />

odor-active compounds in fresh and dried hop cones<br />

(Humulus lupulus L. variety spalter select) based on<br />

GC-olfactometry and odor dilution techniques. J.<br />

Agric. Food Chem. 2000, 48, 1776-1783.<br />

[3] De Keukeleire, D.; David, F.; Haghebaert, K.; Sandra,<br />

P. Automated reporting on the quality of hops and hop<br />

products.; J. Inst. Brew. 1998, 104, 75-82.<br />

[4] Irwin, A. J. Varietal dependence of hop flavour volatiles<br />

in lager. J. Inst. Brew. 1989, 95, 185-194.<br />

[5] Goiris, K.; De Ridder, M.; De Rouck, G.; Boeykens,<br />

A.; Van Opstaele, F.; Aerts, G.; De Cooman, L.; De<br />

Keukeleire, D.; The oxygenated sesquiterpenoid<br />

fraction of hops in relation to the spicy hop character<br />

of beer. J. Inst. Brew. 2002, 108, <strong>86</strong>-93.<br />

[6] Lermusieau, G.; Bulens, M.; Collin, S. Use of GC-olfactometry<br />

to identify the hop aromatic compounds in<br />

beer. J. Agric. Food Chem. 2001, 49, 3<strong>86</strong>7-3874.<br />

Toru Kishimoto and co-workers in the<br />

Asahi R&D Centre laboratories.<br />

ole, myrcene, -caryophyllene and -farnesene),<br />

123 (-citronellole and humulen epoxide<br />

I), 149 (-eudesmole), 177 (-damascenone,<br />

internal standard) and 190 (-damascone).<br />

Thermal desorption and GC/MS method<br />

parameters<br />

Flavor compounds concentrated in the Twister<br />

PDMS phase were subsequently thermally desorbed<br />

in the <strong>GERSTEL</strong> TDU using the following<br />

temperature program: Initial temp. 25 °C,<br />

hold time 0 min, ramp rate 2.5 °C/min to 240 °C,<br />

hold time 5 min. Analytes were refocused in the<br />

<strong>GERSTEL</strong> CIS at –100 °C using LN2 cooling;<br />

CIS Mode: splitless. At the start of the GC/MS<br />

run, the CIS temperature program was started,<br />

releasing the focused analytes to the GC column.<br />

CIS program: Initial temp. –100 °C; hold<br />

time 0 min; ramp rate 2 °C/min to 240 °C; hold<br />

time 5 min. GC/MS parameters were identical to<br />

those listed above under liquid extraction with<br />

dichloromethane.<br />

[7] David, F.; Sandra, P.; Hoffmann, A.; Harms, D.;<br />

Nietzsche, F.; Elucidation of the Hoppy Aroma in<br />

Beers by Stir Bar and Headspace Sorptive Extraction<br />

followed by Thermal Desorption – CGC-MS/PFPD:<br />

http://www.gerstel.com/an_2001_04.htm (accessed<br />

30th May 2005), Gerstel Application <strong>No</strong>tes<br />

4/2001.<br />

[8] Demyttenaere, J. C. R.; Sanchez Martinez, J. I.; Verhe,<br />

R.; Sandra, P.; De Kimpe, N. Analysis of volatiles of<br />

malt whisky by solid-phase microextraction and<br />

stir bar sorptive extraction. J. Chromatogr. 2003,<br />

985, 221-232.<br />

[9] King, A. J.; Dickinson, J. R. Biotransformation of hop<br />

aroma terpenoids by ale and lager yeasts. FEMS<br />

Yeast Res. 2003, 3, 53-62.<br />

[10] Maylan, M. W.; Howard, P. H. Atom/Fragment contribution<br />

method for estimating octanol-water partition<br />

coefficients. J. Pharm. Sci. 1995, 84, 83-92.<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

7


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Service<br />

<strong>GERSTEL</strong> MAESTRO Software<br />

Virtuosity Defined<br />

The <strong>GERSTEL</strong> MAESTRO software provides harmonious and efficient<br />

integrated control of <strong>GERSTEL</strong> modules and solutions. MAESTRO was<br />

introduced in early 2006, replacing the established MASter software;<br />

MAESTRO provides significant improvements in flexibility and ease-ofuse,<br />

both in method generation and in the analysis sequence set-up.<br />

Ease-of-use ultimately translates to less errors, less time spent setting up<br />

analyses, and improved lab productivity. <strong>GERSTEL</strong> gratefully acknowledges<br />

our customers contributions.By providing valuable insights and suggestions<br />

they have made MAESTRO software more useful in the laboratory<br />

environment. In this article, we would like to show how MAESTRO helps to<br />

quickly and easily set up analyses, simplifying and speeding up your every<br />

day activities in LC/MS and GC/MS<br />

The author<br />

Sabine Fischer<br />

<strong>GERSTEL</strong> GmbH & Co. KG<br />

Aktienstraße 232 – 234<br />

45473 Mülheim an der Ruhr<br />

sabine_fischer@gerstel.de<br />

8<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Service<br />

How to conduct yourself in a new software environment<br />

<strong>GERSTEL</strong> MAESTRO step-by-step<br />

To give you a clear view of the efficiency<br />

and ease-of-use of MAESTRO software<br />

operation, this article will provide a<br />

step-by-step guide on how to set up a method.<br />

Even with little or no experience from<br />

MAESTRO’s predecessor, the MASter software,<br />

you will be able to familiarize yourself<br />

with MAESTRO very quickly.<br />

Whatever the task at hand and no matter<br />

which system configuration you have:<br />

The detailed, easy-to-use MAESTRO-online<br />

help guides you all the way. Help topics<br />

are divided into chapters and sections similar<br />

to the structure of an operator’s manual.<br />

The information is easily accessed, providing<br />

answers to your questions concerning<br />

software handling in a clear and concise<br />

manner, in English, German or Japanese.<br />

Several convenient ways to<br />

find help and information:<br />

Accessing on-line help<br />

There are several easy ways to find information<br />

when you need it. You can either<br />

select the menu item Help – Help Topics –<br />

<strong>GERSTEL</strong> MAESTRO from the menu line,<br />

opening the start page of online help, or you<br />

simply click on the help button in the input<br />

window. Context-sensitive on-line help<br />

is available, just place the cursor on an input<br />

field or button and push the F1 key. In<br />

this case, help pages appear with information<br />

on the selected element.<br />

Method step-by-step<br />

To demonstrate the set-up in practice, the<br />

following example shows step-by-step how<br />

to generate a method. The example is for<br />

the Cooled Injection System (CIS) GC inlet<br />

combined with liquid injection based on<br />

the MultiPurpose Sampler (MPS).<br />

Step 21<br />

Select Sampler<br />

<strong>No</strong>w select the MPS as sampler; when the<br />

MPS has been selected you can select the<br />

relevant parameters for liquid injection.<br />

For this purpose, select the menu item<br />

<strong>GERSTEL</strong> – Select Sampler from the menu<br />

line. The window Select Sampler opens.<br />

Select MPS from the list.<br />

Step 31<br />

Parameters for liquid<br />

injection<br />

From the menu bar, select the menu item<br />

<strong>GERSTEL</strong> – Edit <strong>GERSTEL</strong> Parameters.<br />

The window <strong>GERSTEL</strong> Parameters opens<br />

up, displaying the parameters System Settings.<br />

At the bottom left, click on the MPS<br />

button. The parameters for liquid injection<br />

are shown on the tab page Liquid Injection<br />

Settings. Enter the required method<br />

parameter values. If you want to add<br />

rinse steps, to rinse the syringe between injections,<br />

click on the tab Rinse Settings –<br />

this will open up the page with rinse parameters.<br />

Indicate for each type of rinse, when it<br />

must take place and from which wash vial<br />

the rinse solvent should be taken. Preclean<br />

rinses, as the name implies, are performed<br />

prior to injection, post-clean, after<br />

the injection. Please note: Rinsing with<br />

sample can only be selected for pre-clean,<br />

not for post-clean.<br />

<strong>No</strong>w please<br />

switch to the<br />

CIS page.<br />

Step 41<br />

Enter CIS parameters<br />

At the top left, click on the CIS button and<br />

the method parameters for the CIS are displayed;<br />

enter the desired CIS parameters.<br />

Should a parameter value lie outside the<br />

permitted range, the software will respond<br />

with a warning. If the parameter value is<br />

changed to fall within the allowed range,<br />

the software will accept the value. By clicking<br />

OK, the parameters are accepted and are<br />

uploaded to the controller. The CIS is now<br />

ready to start. Close the window.<br />

Step 51<br />

Save method<br />

<strong>No</strong>w all you have to do is save the parameters<br />

in a named method, which you can load<br />

again later and use as basis for the analysis<br />

sequence. Save and name the method<br />

and then proceed as you would normally<br />

do when working with the ChemStation<br />

without integrated MAESTRO software.<br />

You are now ready to go!<br />

Select CIS with the mouse to set the parameters<br />

of the Cooled Injection System (CIS).<br />

Step 11<br />

Start MAESTRO<br />

Let’s assume you work with the Agilent<br />

Technologies ChemStation software.<br />

When you start ChemStation, the integrated<br />

MAESTRO software is automatically<br />

started in the background. Switch on<br />

all hardware components before starting<br />

the software.<br />

Parameters for the liquid injection can only<br />

be set after you have selected Multi Purpose<br />

Sampler (MPS). Otherwise, the MPS parameter<br />

window will not be displayed.<br />

The <strong>GERSTEL</strong> MAESTRO software runs in the background when<br />

operating the Agilent Technologies ChemStation software.<br />

MAESTRO can operate with any standard software in “standalone”<br />

mode.<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

9


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Service<br />

By expert users for expert users<br />

<strong>GERSTEL</strong> MAESTRO<br />

Ralf Bremer<br />

As a company that specializes in developing,<br />

manufacturing and supporting instruments<br />

and systems for chemical analysis, <strong>GERSTEL</strong><br />

relies on input from experienced users. Input<br />

is needed in order to constantly offer the best<br />

possible solutions for modern<br />

laboratories. Equally, cooperation<br />

with experienced<br />

beta testers is vital. GER-<br />

STEL has always had cooperation<br />

with users in government<br />

agencies, academia<br />

and industry in order to always<br />

be able to provide advanced and rugged<br />

solutions that are useful in the lab.<br />

“Such collaborations provide a win-win<br />

situation for the parties involved”, says Ralf<br />

Bremer (photo), General Manager, <strong>GERSTEL</strong><br />

R&D and Production. Ultimately, they help<br />

us bring better products and solutions to the<br />

market place; The most recent example is the<br />

Dynamic Headspace (DHS) accessory for the<br />

MultiPurpose Sampler (MPS) (see page 17).<br />

The MAESTRO software development<br />

project was no different. MAESTRO controls<br />

and interacts with all <strong>GERSTEL</strong> modules<br />

and systems. Still, it is easy to configure<br />

and set up – whether in “stand-alone“<br />

mode or integrated with the Agilent Technologies<br />

ChemStation. Fred Schwarzer,<br />

Ph.D., manager of the <strong>GERSTEL</strong> Software<br />

Development Department explains: “We<br />

implemented a long list of customer suggestions<br />

and were able to significantly improve<br />

and expand functionality, efficiency<br />

of operation and ease-of-use.”<br />

Guido Deußing<br />

Editor<br />

If you have questions<br />

about the MAESTRO<br />

Software, whether about<br />

functions, configurations<br />

or any other items of<br />

interest, please mail us<br />

at gerstel@gerstel.com.<br />

MAESTRO offers<br />

freedom of entry and<br />

freedom of selection<br />

The method parameters that must be entered<br />

to set up a method depend on the<br />

configuration and on the task at hand. How<br />

much time and effort is needed to set up<br />

a method depends not only on the complexity<br />

of the analysis, but also on the system<br />

you use.<br />

MAESTRO makes your life easy: parameters<br />

can be directly selected by mouse<br />

click and filled in - or the method editor can<br />

simply take you through all parameters step<br />

by step until all entries have been made<br />

and the method completed. Whenever the<br />

mouse cursor is placed over a parameter<br />

entry field, a text field with a short explanation<br />

pops up to make it as easy as possible<br />

to fill in the parameter correctly. For<br />

example, if you place the mouse cursor on<br />

the Initial Temperature entry field, the valid<br />

range is automatically displayed: min: -150<br />

°C to max: 400 °C. For more detailed info,<br />

just highlight an entry field and press F1 to<br />

get full context-sensitive help.<br />

Explanations<br />

about each<br />

parameter can<br />

be accessed<br />

via contextsensitive<br />

help.<br />

For more information<br />

about the MAESTRO<br />

software, please visit our<br />

website at www.gerstel.<br />

com or contact your local<br />

<strong>GERSTEL</strong> representative.<br />

10<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Service<br />

1<br />

Generating sequences<br />

Easier than ever<br />

<strong>GERSTEL</strong> is using the slogan “Sample Prep by mouseclick”<br />

to let the world know how easy it is to operate<br />

our equipment with the MAESTRO software. This is<br />

best illustrated by an example, demonstrating the minimal<br />

efforts required to complete the sequence table to<br />

Fred Schwarzer, Ph.D.<br />

run your daily samples.<br />

This otherwise tedious and time consuming procedure<br />

is handled by the MAESTRO software with literally just a few mouseclicks.<br />

Dr. Fred Schwarzer (pictured), head of <strong>GERSTEL</strong> software development:<br />

“The user simply marks the complete sequence line and enters via<br />

the repeat button, how often the line is to be repeated.“ [Screenshot 1]<br />

If only one cell is marked, pushing the repeat button will repeat this<br />

cell as many times as indicated by the user. “This is very practical for replacing<br />

trays, injectors or methods within an existing sequence table”, says<br />

Fred Schwarzer. [Screenshot 2]<br />

Simply cut, paste and complete<br />

The sequence table supports copy/paste functions [Screenshot 3]. Additionally,<br />

the Auto-complete function can be activated. Dr. Fred Schwarzer: “If the<br />

user enters the sample name, it is automatically completed after entering the<br />

first few letters, just as you know it from the Microsoft® Excel software.“<br />

In the sequence table, methods, trays and injectors can be selected<br />

directly from pull-down menus. According to Dr. Schwarzer „only those<br />

methods that are configured with the selected syringe are displayed. This<br />

makes method selection easier and reduces the risk of error“. [Screenshot 4]<br />

The same applies to trays and injectors: It is only possible to select those<br />

that fit the method listed in the sequence line.<br />

2<br />

3<br />

Intelligent fill-down<br />

Last, but not least, you can specify in the Checkbox “Increment Vial/Datafile”<br />

whether you want the vial number and data file name to be incremented<br />

automatically when repeating rows or cells via the repeat button.<br />

4<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

11


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Report<br />

To perfect the composition of a wine, scientists start<br />

by separating the score of flavors into single notes.<br />

In their quest for a bouquet of fragrant high notes,<br />

scientists at the Research Institute Geisenheim rely<br />

on some rather unusual methods.<br />

Lab on the slopes<br />

Flavor from trash cans<br />

In a German vineyard, scientists of the Research<br />

Institute of Geisenheim practice an<br />

unusual, but very sophisticated type of viticulture<br />

using hundreds of trash cans. The<br />

Geisenheim wine researchers are systematically<br />

pursuing the lofty goal of creating perfectly<br />

balanced wine. They must follow an intricate<br />

path so that factors which could influence<br />

the taste or cause off-odor is addressed<br />

in the vineyard, not in the cellar.<br />

ficial quality inspection: „We want to find<br />

out why lately, in some German white wines<br />

such as Riesling, Kerner and Müller-Thurgau<br />

an off-odor develops with increasing<br />

age” explains Prof. Otmar Löhnertz.<br />

The expert oenologist explains that the<br />

trash cans are used to better observe the<br />

complicated wine system and to influence<br />

the development of plants and grapes by<br />

changing various parameters.<br />

“In the trash cans, we investigate the development<br />

of the vines by specifically varying<br />

the intensity of sunlight, the supply of<br />

nutrients and the precipitation”, says Prof.<br />

Löhnertz. „We now strongly suspect that<br />

climatic stress is the cause of UTA.“<br />

A plant is stressed by factors such as<br />

strong UV radiation, high temperatures<br />

like those experienced in Europe in the<br />

summer of 2003, and by a shortage of nutrients<br />

in the soil. The undesirable flavor<br />

that can originate from stress conditions is<br />

formed by young wine just a few months<br />

after fermentation. In small doses, 1-AAP<br />

»We suspect that<br />

climatic stress is<br />

the cause of the<br />

atypical aging<br />

(UTA) off-odor.«<br />

Prof. Otmar Löhnertz,<br />

Research Institute<br />

Geisenheim<br />

Searching for off-odors<br />

A white wine contains 800 to 1000 different<br />

taste and flavor components, a red<br />

wine even more. In their laboratories, the<br />

Geisenheim scientists try to break down the<br />

flavor into its individual components. Most<br />

recently, they identified „atypical aging flavor“<br />

(UTA), which is caused by the presence<br />

of 2-aminoacetophenone (2-AAP). Wines<br />

containing 2-AAP are flat and appear excessively<br />

aged with a distinct fragrance note<br />

of mothballs. It has been due to the 2-AAP<br />

that some Riesling wines didn’t pass the ofis<br />

a pleasant flavor with a fruity note. Increase<br />

the dose, however, and the unpleasant<br />

“mothball” odor comes to the forefront.<br />

The “aging” flavor is not only found in German<br />

vineyards, this research will apply to all<br />

wines that have problems with UTA.<br />

<strong>No</strong>t every grape variety is<br />

right for every vineyard<br />

From a scientific point of view, wine quality<br />

depends mainly on two initial factors:<br />

12<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Report<br />

tion, winegrowers must be familiar with the<br />

wine’s flavor compounds, and how these<br />

are formed based on both soil conditions<br />

and microclimate. Once these<br />

substances are determined, and<br />

the mechanism on how they are<br />

generated is known, their formation<br />

can be directly influenced.<br />

Additionally, if a winegrower<br />

sets out to produce<br />

top quality wines, he must<br />

reduce the crop size.<br />

The idea behind this is<br />

simple: The flavor compounds<br />

that are generated<br />

by the vines are<br />

shared between fewer<br />

grapes and so they<br />

are available in higher<br />

concentrations; in<br />

turn, the flavor of each<br />

grape becomes more<br />

pronounced.<br />

„We are trying to optimize<br />

the fruit flavor“, says Prof. Löhnertz.<br />

When leaves are removed from the<br />

Riesling vines, for example, the grapes are<br />

exposed to more sunlight which helps produce<br />

larger amounts of the compounds that<br />

are responsible for the fruity flavor. However,<br />

mistakes and pitfalls must be avoided<br />

in many parts of the process.<br />

Otmar Löhnertz mentions that winegrowers<br />

often seek his advice on how to address<br />

risks to product quality. „We are especially<br />

contacted by winegrowers that lack<br />

the chemical analysis capabilities in their<br />

cellars.”<br />

climate and soil conditions. Thus, winegrowers<br />

have to carefully consider<br />

which grape varieties are best suited<br />

for their growing area. Planting<br />

a Riesling in a warm climate zone,<br />

like California or South Africa,<br />

would result in significantly<br />

less flavor compounds being<br />

formed. The wine would never<br />

develop the characteristic<br />

fruity freshness. Red wines,<br />

on the other hand, have difficulties<br />

in Germany, even<br />

though the hot summer<br />

of 2003 prompted renewed<br />

discussion on<br />

whether it would be<br />

possible to cultivate<br />

a strong, full-bodied<br />

red wine in northern<br />

regions as well.<br />

Quality at<br />

the expense of<br />

quantity<br />

The soil type in which a vine<br />

grows in part determines the<br />

flavor of a wine. But, by what<br />

mechanism does this happen?<br />

To answer this ques-<br />

Analyzing flavors is like decomposing<br />

a musical score<br />

into single notes.<br />

The Geisenheim Research Institute maintains<br />

a number of laboratories dedicated to<br />

flavor analysis. Researchers inject flavor extracts<br />

of wines into high resolution gas chromatography<br />

systems, trying to determine<br />

every nuance of the extract by separating<br />

it into hundreds of individual components.<br />

It is like decomposing a large musical score<br />

into single notes: high or low, dominant or<br />

subtle. The only difference is that this performance<br />

is not rendered by musicians, but<br />

by chemists, who sniff out the flavor note<br />

and assign a sensory attribute to each molecule.<br />

In doing so, it is possible to link chemical<br />

analysis with olfactory sensing in an ideal<br />

way, enabling sensory wine analysis.<br />

The effluent from the GC column is<br />

split so that it arrives simultaneously at the<br />

nose and at another detector, usually a mass<br />

spectrometer since it is capable of specific<br />

compound identification. The compounds<br />

are presented to the nose through the use<br />

of an Olfactory Detector Port (ODP), and<br />

trained personnel determine the identity<br />

and intensity of the flavor compounds<br />

both of which are recorded as part of the<br />

analytical data file.<br />

Wine flavors dictated<br />

by the market<br />

GC/ODP analysis can help to understand<br />

the flavor composition of good wines, but<br />

can of course also be used when products<br />

are recreated “synthetically”, helping<br />

to create flavors with popular appeal<br />

for mass market consumption. According<br />

to the Geisenheim experts, international<br />

mass markets seem to require less personality<br />

than ever. Instead, global trends are<br />

set by wine gurus like the French oenologists<br />

Michel Rolland, who is a dominating<br />

figure in wine circles on every continent<br />

and by the American Robert Parker. A winery,<br />

whose product receives a positive review<br />

in Parker’s Wine Advocate magazine,<br />

can pop the Champagne corks and celebrate.<br />

Such is the critic’s influence on the<br />

market. Hence, many wine makers comply<br />

with Parker’s preferences. In this case,<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

13


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Report<br />

profit rules the market and dictates taste;<br />

science becomes the tool to help tailor the<br />

wine to meet the trend. Slightly more black<br />

currant flavor here, a little more freshness<br />

there: Currently, fruity, moderately sparkling<br />

wines are popular. These can be produced<br />

by growing wine under cooler conditions<br />

at higher elevations or by fermenting<br />

the grape juice at lower temperatures.<br />

Many wine growers consider wine design<br />

that follows such market requirements<br />

a potential problem. What limits should we<br />

impose on wine design? The limits of most<br />

in the industry were certainly crossed when<br />

employees of a South African winery added<br />

bell pepper flavor to the wine. To most wine<br />

professionals, adulterating wine with flavors<br />

foreign to the species is nothing short<br />

of sacrilege. Some companies have contemplated<br />

diluting strong red wines with water<br />

since customers are less interested in wines<br />

with high alcohol levels. In Geisenheim,<br />

stricter rules apply concerning the limits<br />

for designer wines. „If this trend continues,<br />

we will approach a situation where only<br />

synthetic mass products are available”, says<br />

Klaus Schaller, head of the research institute.<br />

The thought is clearly not appealing<br />

to the seasoned oenologist.<br />

A seasoned gut feeling<br />

and intuition to hit that<br />

special note<br />

Then what is the noble art of wine making?<br />

First of all, it requires expertise on the effects<br />

of growing conditions, sunlight, and<br />

soil quality, susceptibility to diseases, fungi<br />

and pests. „When it comes to the really<br />

important decisions, I use my gut feeling:<br />

You cannot produce a good wine without<br />

a healthy dose of creativity“, says Rowald<br />

Hepp, who grows only Riesling in his<br />

vineyard “Schloss Vollrads”, according to<br />

the magazine ‘Capital’ among the top one<br />

hundred in the world. „To create wine with<br />

individual personality, you need to go beyond<br />

science and call on your intuition“,<br />

says Carlos Moro, a winegrower from<br />

Spain.<br />

For amateurs, the basics may be comprehensible:<br />

Taste and flavor is controlled<br />

by maturing the wine in a barrel under<br />

the influence of yeast. The details of how<br />

to influence the fermentation to provide<br />

top wines, however, is still more of an art<br />

than a science, understood only by master<br />

wine makers, each with his or her well<br />

kept secrets.<br />

If wine growers are forced to conform<br />

to mass market tastes, “the<br />

growers and wine makers that thrive<br />

on authenticity will not survive in the<br />

long run”, warns Klaus Schaller.<br />

Just a single evening spent in good<br />

company sampling a wide variety of<br />

wines served in proper glasses can<br />

give you an impression of the word<br />

“authentic”, and why it is worth preserving.<br />

<strong>GERSTEL</strong> Olfactory Detector Port ODP<br />

Visualizing odor intensities<br />

Identifying flavor compounds or compounds that cause offodors<br />

are tasks that quickly expose the limitations of standard<br />

instruments and methods. The <strong>GERSTEL</strong> Olfactory Detector<br />

Port (ODP) allows sensing of compounds by the human nose<br />

as they elute from the column of a gas chromatograph, but<br />

the most powerful means of identifying flavors, fragrances<br />

and off-odors incorporates the addition of a mass spectrometer.<br />

For this technique, the effluent is split as it leaves the<br />

column so that it arrives simultaneously at the nose and the<br />

mass spectrometer, providing both sensory and chemical<br />

identification.<br />

A voice recognition software package provides a detailed<br />

“olfactogram” that includes odor intensity, retention<br />

time and voice comments for compounds as they elute. All<br />

data is stored with the Agilent ChemStation results and can<br />

be presented in a number of different ways. Among these<br />

are overlapping chromatograms and olfactograms and data<br />

reports with descriptors, that help with data interpretation<br />

and problem solving.<br />

14<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Distributor<br />

TEGENT TECHNOLOGY LTD.<br />

(HEAD OFFICE)<br />

Room 2103-05, Westin Centre<br />

26 Hung To Road<br />

Kwun Tong, Kowloon – Hong Kong<br />

P.R. China<br />

Tel. +852 27 - 59 21 82<br />

Fax +852 27 - 58 38 30<br />

tegent@netvigator.com<br />

hko@tegent.com.cn<br />

GUANGZHOU OFFICE<br />

Room 1505;15th floor;<strong>No</strong>219 CTS<br />

Center; Zhong Shan Wu Road, Guangzhou<br />

510030, P.R. China<br />

Tel. +020 - 22273388<br />

Fax +020 - 22273368<br />

guangzhou@tegent.com.cn<br />

BEIJING OFFICE<br />

Room 306, Kunxun Tower, <strong>No</strong>.9,<br />

Zhichun Road, Haidian District, Beijing,<br />

100083 , P.R. China<br />

Tel. +010 - 82327383/8992<br />

Fax +010 - 82329551<br />

beijing@tegent.com.cn<br />

Tegent Technology Ltd.<br />

<strong>GERSTEL</strong> Distributor for China<br />

Tegent is a leading provider of high technology<br />

instrumentation and services for<br />

analytical laboratories in China. The company<br />

was established in Hong Kong in 1992.<br />

Today, Tegent has about 140 staff in 11 offices<br />

throughout China including 2 laboratories<br />

for demonstrations and technical<br />

support.<br />

Your contact<br />

Bernd Wiesend<br />

International Sales Manager<br />

<strong>GERSTEL</strong> GmbH & Co. KG<br />

Aktienstrasse 232 - 234<br />

D-45473 Mülheim a. d. Ruhr, GERMANY<br />

Phone: + 49 (208) 7 65 03-0<br />

bernd_wiesend@gerstel.de<br />

Partners<br />

In 2001, Tegent became an official distributor<br />

for <strong>GERSTEL</strong> with exclusive rights to<br />

distribute <strong>GERSTEL</strong> products throughout<br />

China. Tegent represents Agilent Technologies<br />

in Hong Kong and is an Authorized<br />

Service Provider (ASP) for Agilent<br />

throughout China. These facts made the<br />

partnership between Tegent and <strong>GERSTEL</strong><br />

especially attractive since <strong>GERSTEL</strong> is the<br />

leading Premier Solution Partner of Agilent<br />

Technologies world-wide.<br />

Tegent currently has around 5,000 customers,<br />

covering many markets: From government<br />

departments, environmental protection<br />

agencies and universities through<br />

chemical, petrochemical, pharmaceutical,<br />

tobacco and food producing companies to<br />

commercial testing laboratories.<br />

With a nation-wide network of offices<br />

and staff, Tegent is well positioned as preferred<br />

partner for many national and international<br />

customers, providing high quality<br />

instrumentation along with reliable and<br />

effective services. From sample preparation<br />

to chemical analysis using a number<br />

of chromatographic and other techniques,<br />

Tegent provides complete solutions.<br />

SHANGHAI OFFICE<br />

Units 1901-1902, Yin Fa Mansion,<br />

<strong>No</strong>. 1068 West Beijing Road, Shanghai,<br />

200041, P.R. China<br />

Tel. +021 - 52610159<br />

Fax +021 - 52610122<br />

shanghai@tegent.com.cn<br />

CHENGDU OFFICE<br />

Room 721, Li du Mansion, <strong>No</strong>.8 DaKeJia<br />

Xiang, Chun Xi Road, Chengdu,Sichuan,<br />

610016 , P.R. China<br />

Tel. +028 - <strong>86</strong>656745/46/47<br />

Fax +028 - <strong>86</strong>656744<br />

chengdu@tegent.com.cn<br />

NANNING OFFICE<br />

Room 09, Floor 18, Tai An Tower, <strong>No</strong>. 38-2<br />

Min Zu Avenue, Nanning, Guangxi,<br />

530022, P.R. China<br />

Tel. +0771 - 5890482/25 5892224<br />

Fax +0771 - 5890402<br />

nanning@tegent.com.cn<br />

XIAMEN OFFICE<br />

Unit 15A2BC, Huang-da Tower,<br />

<strong>No</strong>. 28 Hou-dai-xi Road, Xiamen, Fujian,<br />

361004, P.R. China<br />

Tel. +0592 - 5185885/751/835<br />

Fax +0592 - 51858<strong>86</strong><br />

xiamen@tegent.com.cn<br />

KUNMING OFFICE<br />

Room 906, Green Land Building, <strong>No</strong>.80<br />

Tuo Dong Road, KunMing, YunNan.<br />

650041, P.R. China<br />

Tel. +0871 - 3157061/021/<br />

136/211/170<br />

Fax +0871 - 3157015<br />

kunming@tegent.com.cn<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

15


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide innovation<br />

Automated<br />

Tube EXchange<br />

(ATEX)<br />

Automated Tube EXchange<br />

(ATEX) has been introduced for<br />

the <strong>GERSTEL</strong> MultiPurpose<br />

Sampler (MPS) in combination<br />

with the <strong>GERSTEL</strong> Thermal Desorption Unit (TDU).<br />

The ATEX option enables the introduction of liquid<br />

samples directly into micro-vial inserts used for<br />

thermal desorption / thermal extraction in the TDU.<br />

Extracted analytes are refocused and concentrated<br />

in a Cooled Injection System (CIS) inlet prior to<br />

introduction to the GC/MS system. The efficient<br />

extraction and concentration ensures highest<br />

possible sensitivity and lowest detection limits.<br />

The analysis system is kept free of high-boiling<br />

contaminants and matrix residue ensuring best<br />

possible stability and system uptime.<br />

The ATEX micro-vials can be used for liquid or<br />

solid samples. Up to 196 samples can be processed<br />

automatically for determination of VOC / SVOC in<br />

heavy or involatile matrices. Following the analysis,<br />

the sample cup with the remaining high-boiling or<br />

solid residue is automatically removed. ATEX helps<br />

to ensure maximum uptime and best possible analysis<br />

results by keeping involatile or complex matrix<br />

material out of the GC/MS system. Standard addition<br />

and other liquid phase sample preparation steps can<br />

be performed automatically by the MPS. The complete<br />

system is controlled directly from the <strong>GERSTEL</strong><br />

MAESTRO software or integrated with the Agilent<br />

ChemStation. Just one method and one sequence<br />

table controls the complete process from Sample<br />

Introduction through thermal desorption to GC/MS<br />

analysis ensuring the simplest possible operation.<br />

Suggested Applications<br />

Determination of VOC or SVOC in high-boiling or involatile<br />

matrices by thermal extraction, also referred<br />

to as dynamic headspace analysis or stripping. Examples<br />

are: gasoline in engine oil, plasticizers from<br />

packaging material in foods and edible oils, and fragrance<br />

compounds used in household products or<br />

personal care products. <br />

Highlights<br />

PittCon 2007<br />

At the Pittsburgh Conference 2007, held in Chicago,<br />

Illinois, <strong>GERSTEL</strong> presented new products and<br />

applications. The main focus was on automated<br />

sample preparation and sample introduction for GC<br />

and LC. The main news briefs are presented here.<br />

Automated SPE<br />

<strong>GERSTEL</strong> has introduced automated Solid<br />

Phase Extraction (SPE) for the MultiPurpose<br />

Sampler (MPS). The system is based<br />

on standard cartridges, using disposable<br />

needles for liquid transfer to eliminate carry-over.<br />

Users can work on a variety of sample<br />

types due to the flexible rinse and elution<br />

capabilities offered by the MPS. It is<br />

possible to combine automated SPE with<br />

sample prep steps and with introduction<br />

to LC/MS or GC/MS systems. By performing<br />

SPE and chromatography in parallel,<br />

productivity can be optimized. The complete<br />

system is controlled by the <strong>GERSTEL</strong><br />

MAESTRO software or integrated with the<br />

Agilent Technologies ChemStation. <br />

Liquid<br />

introduction<br />

(LC)<br />

High<br />

Throughput<br />

Automated<br />

Sample<br />

Preparation<br />

Heated or<br />

cooled<br />

sample trays<br />

Automated Solid<br />

Phase Extraction<br />

(SPE)<br />

16<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Innovation<br />

GC<br />

PrepStation<br />

The <strong>GERSTEL</strong> MPS Prep-<br />

Station automates a wide range of GC sample preparation<br />

and sample introduction techniques. Liquid<br />

sample preparation, such as standard addition, derivatization<br />

and extraction, is combined with liquid,<br />

headspace or SPME sample introduction. Sample<br />

preparation is performed during GC analysis of the<br />

preceding sample for maximum throughput. The<br />

PrepStation is controlled from the Agilent Technologies<br />

ChemStation software using <strong>GERSTEL</strong> MAE-<br />

STRO software PrepBuilder functions. One method<br />

and one sequence table operate the complete system<br />

– from sample preparation and sample introduction<br />

to GC and GC/MS analysis. The PrepStation and<br />

<strong>GERSTEL</strong> MAESTRO software operate conveniently<br />

with any standard GC system. <br />

Automated Dynamic Headspace Option<br />

An automated Dynamic Headspace (DHS)<br />

option has been introduced for the <strong>GERSTEL</strong><br />

MultiPurpose Sampler (MPS) based on<br />

newly developed technology.<br />

A DHS station is used to efficiently extract<br />

and concentrate VOCs from liquid or<br />

solid samples placed in standard headspace<br />

vials. The DHS station provides thermostating<br />

and agitation as well as purging of<br />

the sample headspace with inert gas. Sample<br />

temperatures can be selected from 200 °C<br />

to as low as 10 °C, enabling control of the<br />

amount of water vapor released and ultimately<br />

retrapped. The DHS station additionally<br />

holds a replaceable adsorbent- or<br />

sorbent filled tube used for analyte concentration.<br />

The temperature of the adsorbent<br />

tube during the DHS process can be varied<br />

from 20 °C to 70 °C for optimal trapping of<br />

the analytes of interest.<br />

Adsorbent tubes used are standard<br />

<strong>GERSTEL</strong> Thermal Desorption Unit (TDU)<br />

tubes. Following analyte concentration, the<br />

tube is automatically transferred to the TDU<br />

for thermal desorption and analyte transfer<br />

to the GC. Tubes are fitted with individual<br />

adapters enabling<br />

both automated movement<br />

and leak-free sealing<br />

during the DHS and<br />

thermal desorption<br />

steps and during storage<br />

in the auto-sampler<br />

tray.<br />

Automated liquid<br />

handling in the MPS<br />

can be used for additional<br />

sample preparation<br />

steps. As part of<br />

the sample preparation<br />

procedure, standard<br />

addition can be<br />

performed automatically<br />

for best possible analytical results. Automated<br />

DHS combined with sample introduction<br />

to a GC or GC/MS system is performed<br />

by the MPS and TDU. Up to 98 samples<br />

can be processed automatically in one<br />

sequence.<br />

Parallel processing of samples enable<br />

the DHS process to be performed during<br />

the chromatographic run of the preceding<br />

sample for optimal productivity<br />

and for highest<br />

system utilization. Sample<br />

prep steps are selected<br />

by mouse-click from<br />

a pull-down menu using<br />

the PrepBuilder function<br />

of the <strong>GERSTEL</strong><br />

MAESTRO software.<br />

A graphical scheduler<br />

display for the<br />

DHS process provides<br />

an overview of the time<br />

required for each individual<br />

step and for the<br />

complete sequence of<br />

samples for easier planning.<br />

Just one method and one sequence<br />

table controls the complete process from<br />

DHS through sample prep and sample introduction<br />

to GC/MS analysis. Integrated<br />

control ensures a more efficient operation<br />

with less risk of error. The <strong>GERSTEL</strong><br />

MAESTRO software operates stand-alone<br />

or fully integrated with the Agilent Technologies<br />

ChemStation software. <br />

Twister<br />

Back<br />

Extraction<br />

(TBE)<br />

PrepAhead –<br />

Saving time by<br />

overlapping sample prep<br />

and GC or LC analysis<br />

Membrane<br />

Assisted Solvent<br />

Extraction<br />

(MASE)<br />

Modular<br />

design, easily<br />

upgradeable<br />

Dynamic<br />

Headspace<br />

System (DHS)<br />

Modular<br />

Accelerated<br />

Column Heater<br />

(MACH)<br />

Solid Phase<br />

Micro<br />

Extraction<br />

(SPME)<br />

Automated<br />

Twister<br />

Option<br />

Headspace<br />

(HS)<br />

Liquid<br />

introduction<br />

(GC)<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

17


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

Health and Food Safety<br />

Fast and reliable<br />

answers regarding<br />

aflatoxins in foods<br />

If you are going to determine the concentration of mycotoxins in<br />

foods, in pharmaceutical products, or in raw materials used in their<br />

production, you will probably rely on Solid Phase Extraction (SPE)<br />

combined with LC/MS analysis. This approach ensures that detection<br />

limits will be lower than the maximum concentrations allowed by<br />

law. While long-established manual SPE procedures may leave little<br />

room for further optimization, automation of the process can provide<br />

laboratories with more reliable results in less than half the time.<br />

The well-stocked cheese counter may<br />

seem to tell a different story, but whoever<br />

consumes moldy foods – other<br />

than mold cheese – is putting his or her<br />

health at risk. This is due to mycotoxins:<br />

Toxins that are created as metabolites by certain<br />

molds. Mycotoxins can lead to acute<br />

illness as well as chronic ailments, caused<br />

by carcinogenic, mutagenic and hormone<br />

active properties that are especially harmful<br />

to infants and toddlers.<br />

To date, more than 300 mycotoxins,<br />

formed by approximately 250 mold types,<br />

have been found. For food safety purposes,<br />

however, only a few mycotoxins are of<br />

importance, such as those of the genus Aspergillus<br />

flavus and Aspergillus parasiticus.<br />

These molds thrive, especially under humid-warm<br />

conditions, on oily and starchy<br />

seeds such as peanuts, walnuts, hazelnuts,<br />

pistachios, almonds, figs, coco, grains, rice,<br />

corn and soy, as well as on dried fruits and<br />

spices.<br />

High concentrations of a group of mycotoxins<br />

called aflatoxins have been found,<br />

for example, in pistachios, figs and cereals.<br />

Aflatoxins are among the most potent human<br />

carcinogens found in plants. The aflatoxins<br />

B1, B2, G1, G2 and M1, produced by<br />

Aspergillus flavus and Aspergillus parasiticus,<br />

belong to the most potent mycotoxins<br />

that exist. Aflatoxin B1 poses the greatest<br />

hazard of all due to its carcinogenic properties.<br />

Because of the extreme toxicity of aflatoxins,<br />

EU legislation specifies very low acceptable<br />

daily intakes and low maximum<br />

residue limits.<br />

The risk of acute poisoning through<br />

high mycotoxin concentrations is relatively<br />

low in most of the developed world thanks<br />

to the overall good food quality. In Africa<br />

and parts of Asia, things can be quite<br />

different: Conditions for growing, storing<br />

and transporting agricultural products are<br />

frequently bad, resulting in moldy peanut<br />

or corn products. Consumption of moldy<br />

products regularly results in acute and even<br />

fatal aflatoxin poisoning. According to literature<br />

references, the lethal dose for an adult<br />

is 1 to 10 mg per kilogram body weight.<br />

Pervasive food contamination<br />

resulted in government regulation<br />

Mycotoxin contamination of food and<br />

feed is a global problem. The UN Food and<br />

Agricultural Organisation (FAO) estimates<br />

that up to 25% of the world’s food production<br />

is contaminated with mycotoxins.<br />

Approximately 20% of the EU‘s cereal harvest<br />

contains detectable amounts of mycotoxins.<br />

Due to the health risk posed by molds<br />

and due to their universal presence in cer-<br />

18<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

Chemical structure<br />

of aflatoxins<br />

Further Information about Aflatoxins<br />

USFDA<br />

http://vm.cfsan.fda.gov/~mow/chap41.html<br />

Cornell University<br />

http://www.ansci.cornell.edu/plants/toxicagents/aflatoxin/aflatoxin.html<br />

Colorado State<br />

http://www.ext.colostate.edu/pubs/CROPS/00306.<strong>pdf</strong><br />

Aflatoxins are a group of more than 20<br />

different fluorescent heterocyclic compounds,<br />

consisting of a dihydro or tetrahydrofuran<br />

unit connected with a substituted<br />

coumarin ring. The toxicologically relevant<br />

compounds are Aflatoxins B1, B2, G1<br />

and G2, with B1 occurring most frequently.<br />

Aflatoxin M1, found for example in milk<br />

and milk products, is a metabolite of Aflatoxin<br />

B1. M1 is formed in humans or in<br />

animals when they have consumed food<br />

or feed contaminated with B1. The toxicity<br />

of Aflatoxin M1 is comparable to Aflatoxin<br />

B1; however, M1 is significantly less<br />

carcinogenic than B1.<br />

tain food products, maximum concentration<br />

values for mycotoxins have been established<br />

in the range of a few micrograms<br />

per kilogram (μg/kg): For peanuts, indehiscent<br />

fruits (mainly nuts), dried fruits and<br />

grain intended for direct consumption or<br />

for use in food products, maximum allowable<br />

concentrations of 2 μg/kg aflatoxin B1<br />

„Fully automated<br />

Solid Phase<br />

Extraction using<br />

the <strong>GERSTEL</strong><br />

SPE system<br />

provides reliable results in<br />

less than half the time it takes<br />

to perform the extraction<br />

manually.” <strong>No</strong>rbert Helle, Ph.D.<br />

or 4 μg/kg total of B1, B2, G1 and G2 apply.<br />

The concentration of aflatoxin M1 in milk<br />

is not allowed to exceed 0.05 μg/kg. Regulations<br />

limit the acceptable quantity in foods<br />

for infants and toddlers to 0.05 μg/kg aflatoxin<br />

B1, and 0.025 μg/kg M1.<br />

Faster results and lower<br />

detection limits<br />

The method of choice for reliable and<br />

sensitive detection of aflatoxins is Solid<br />

Phase Extraction (SPE) or affinity chromatography,<br />

combined with LC/MS analysis.<br />

This approach ensures that detection<br />

limits will be lower than the maximum concentrations<br />

allowed by law.<br />

<strong>No</strong>rbert Helle, Ph.D., food safety analysis<br />

expert and owner of TeLA GmbH, a German<br />

contract laboratory based in Bremerhaven,<br />

explains the background behind<br />

some of his recent work on the determination<br />

of Aflatoxins in foods: „Established<br />

sample preparation methods used in LC/<br />

MS determination of aflatoxin levels provide<br />

only limited scope for optimization,<br />

but reliable and useful analysis results can<br />

be obtained in less than half the time if the<br />

SPE process is automated. In the case of<br />

the aflatoxin determination, manual processing<br />

requires on the order of 4 hours<br />

for eight samples. The <strong>GERSTEL</strong> SPE requires<br />

only 80 to 95 minutes to prepare the<br />

same number of samples, according to Dr.<br />

Helle.<br />

„All steps from standard addition and<br />

derivatization through Solid Phase Extraction<br />

to LC/MS analysis are fully automated”,<br />

says the applications expert, while adding:<br />

“Software-controlled parallel processing<br />

of sample preparation and analysis ensures<br />

that there is only negligible analyte<br />

decomposition. The preparation steps for<br />

each and every sample are performed at exactly<br />

the same point in time prior to analysis.<br />

The <strong>GERSTEL</strong> SPE system provides<br />

on-time sample prep for best possible results”.<br />

Dr. Helle has developed an LC/MS<br />

method for the determination of B1, B2,<br />

G1 and G2 aflatoxins in foods such as pistachios,<br />

bell pepper seasoning and various<br />

fruits. Following clean-up on an SPE affinity<br />

column, the two aflatoxin compounds<br />

O<br />

O<br />

Aflatoxin B1<br />

O<br />

O<br />

O<br />

O<br />

CH 3<br />

O O<br />

Aflatoxin G1<br />

O<br />

O<br />

O<br />

O<br />

O<br />

CH 3<br />

O O<br />

Aflatoxin G2<br />

O<br />

O<br />

O<br />

O<br />

O<br />

CH 3<br />

O<br />

O<br />

Aflatoxin B2<br />

O<br />

O<br />

O<br />

CH 3<br />

O<br />

Brominated aflatoxin B1<br />

O<br />

O<br />

H 3 C Br<br />

O<br />

O<br />

O<br />

O<br />

O<br />

CH 3<br />

Brominated aflatoxin G1<br />

O O<br />

H 3 C Br<br />

O<br />

O<br />

O<br />

O<br />

O<br />

O<br />

CH 3<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

19


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

<br />

Transport sample vial into SPE Vial position<br />

Transport cartridge to the SPE Waste position<br />

<br />

Add 4 mL sample to the cartridge; flow 50 L/s<br />

<br />

Rinse cartridge with 20 mL H2O; flow 50 L/s<br />

PrepBuilder method<br />

for automated SPE. The<br />

MPS is used for sample<br />

preparation to determine the<br />

concentrations of individual<br />

aflatoxins in various food<br />

products such as pistachio,<br />

ground chilli and fruits.<br />

All steps are selected by<br />

mouse-click from a menu<br />

and added to the list.<br />

<br />

<br />

<br />

<br />

<br />

<br />

<br />

<br />

Slide SPE carriage with cartridge from SPE Waste<br />

to SPE Vial position<br />

Elution of aflatoxins with 0.5 mL MeOH;<br />

flow: 30 L/s<br />

Elution of aflatoxins with 0.5 mL MeOH;<br />

flow: 30 L/s<br />

Elution of aflatoxins with 0.5 mL MeOH;<br />

flow: 30 L/s<br />

Wait 30 seconds for the eluent to<br />

transfer completely<br />

Discard SPE cartridge into the cartridge<br />

disposal container<br />

Slide SPE carriage from SPE Vial to<br />

SPE Waste position<br />

Transport sample vial from SPE Vial position<br />

back to tray<br />

<strong>GERSTEL</strong> SPE<br />

Dr. <strong>No</strong>rbert Helle developed his method on an Agilent<br />

Technologies Series 1100 LC/MSD and a <strong>GERSTEL</strong><br />

MultiPurpose Sampler (MPS) with SPE option. The MPS was<br />

also used for derivatization and sample introduction. The<br />

LC/MS system was operated with electrospray ionisation<br />

in positive ion mode. The column used was a Phenomenex<br />

Synergi Max-RP (250*2.1 millimetre, 4 μm particle size)<br />

operated at a flow of 0.3 mL/min. Separation is performed<br />

using a solvent gradient (eluent A: 0.1 % formic acid, eluent<br />

B: acetonitrile). Control of the complete system, from sample<br />

preparation and sample introduction to LC/MS analysis, is<br />

handled from the Agilent Technologies ChemStation software<br />

using the integrated <strong>GERSTEL</strong> MAESTRO software.<br />

with an isolated, non-conjugated, double<br />

bond, B1 and G1, are brominated by stirring<br />

the extract with a 3 % solution of bromine<br />

in chloroform. The mass spectra indicate<br />

that bromination results only in the<br />

formation of 1-methoxy-2-bromo-substituted<br />

compounds. Under the chosen experimental<br />

conditions, dibromo-substituted<br />

aflatoxins are not detected. The 1-methoxy-2-bromo-substituted<br />

compounds<br />

show longer retention times in reversed<br />

phase chromatography than the non-brominated<br />

species, resulting in baseline separation<br />

for the four aflatoxins with minimal<br />

interference from residual matrix. Additionally,<br />

the derivatized compounds yield<br />

significantly better MS responses and the<br />

characteristic bromine pattern in the mass<br />

spectra provides improved differentiation<br />

from background signals and thus a better<br />

signal to noise ratio. These combined<br />

advantages enable the system to reach detection<br />

limits below 0.01 μg/kg for the aflatoxins.<br />

Monobrominated aflatoxins exhibit longer retention times than the nonbrominated<br />

compounds, resulting in better separation of the four aflatoxins and<br />

reduced interference from matrix components (fig. above). Derivatization of<br />

aflatoxins B1 and G1 results in significantly improved MS responses combined<br />

with characteristic bromine patterns in the mass spectra (fig. left):<br />

The detection limits for the examined aflatoxins are below 0.01 μg/kg.<br />

20<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Service<br />

When mycotoxin poisoning is suspected<br />

The Centre for Information To Counter Poisoning,<br />

in the state of <strong>No</strong>rth-Rhine Westphalia,<br />

Germany’s most populous state (population<br />

18 million), is located at the University of<br />

Bonn. Last year, the centre received around<br />

20 calls concerning cases of food poisoning<br />

caused by moldy foods. Cases of acute and<br />

severe poisoning caused by mycotoxin ingestion<br />

are rare. When symptoms call for it,<br />

patients are properly diagnosed by performing<br />

chemical laboratory tests on their blood<br />

serum. When moldy foods are ingested, the<br />

mycotoxins present are absorbed via the digestive<br />

tract and then released into the blood<br />

stream from which they reach the rest of the<br />

body. Aflatoxins are among the most potent<br />

human carcinogens found in plants. Aflatoxin<br />

B1, the most carcinogenic among the mycotoxins<br />

of Aspergillus flavus, unleashes its<br />

effect when metabolized to an epoxide in the<br />

human body. The epoxide attaches itself to<br />

the human genetic material causing potentially<br />

carcinogenic mutations. The accepted<br />

lethal dose of aflatoxin B1 is 1 to 10 mg/kg<br />

bodyweight for adults. Some types of molds<br />

can produce toxins that directly damage the<br />

liver, i.e. these are hepatotoxic.<br />

Moldy foods are in fact spoiled and should be<br />

discarded, not consumed. Exceptions are special<br />

mold cultures used for cheeses, for example,<br />

Camembert, Roquefort, Gorgonzola or Stilton.<br />

Even some specialty Italian salamis can<br />

have been processed using special mold cultures<br />

to provide them with their unique flavor.<br />

White or colored spots are usually a sign of<br />

unhealthy mold growth. The roots of the mold,<br />

also called the mycelium, spread inside the<br />

food, invisible to the naked eye. Both the visible<br />

molds and the mycelium can contain mycotoxins,<br />

such as aflatoxins from Aspergillus flavus,<br />

which has a severe carcinogenic effect.<br />

Fungi spread through the release of spores.<br />

When these reach a nutrient-rich medium, they<br />

can multiply on the surface and/or inside this<br />

medium. Bread, for instance, provides a good<br />

medium for molds. Once the mold is visible at<br />

the surface, it usually has already penetrated<br />

the entire bread. Moldy bread should always be<br />

Typical acute symptoms of aflatoxin poisoning<br />

are digestive problems such as nausea,<br />

diarrhoea and vomiting. Animal experiments<br />

have shown that long-term exposure to aflatoxins<br />

can trigger liver carcinomas; it is widely<br />

assumed that aflatoxins have a similar effect<br />

on humans. The responsible Aspergillus species<br />

appear mainly in nuts and bread.<br />

Exposure to molds can also trigger allergic<br />

reactions, especially in predisposed persons.<br />

The manner in which the mold reaches the organism<br />

would not make a difference, it could<br />

be absorbed via the lungs or digestive tract - or<br />

through contact with skin and mucous membranes.<br />

Health professionals would not refer to<br />

this as a case of poisoning, however.<br />

When mycotoxin poisoning is suspected,<br />

for example when moldy foods have been ingested,<br />

it is recommended to consult a physician<br />

or an organization specialized in helping<br />

patients in cases of poisoning. When mycotoxin<br />

poisoning is diagnosed, frequent tests<br />

of the blood and liver values are performed,<br />

symptomatic therapy of the liver function is<br />

performed, and in some cases medication is<br />

administered to limit uptake of mycotoxins in<br />

the liver. <br />

Scrape off the mold or just throw the food away?<br />

discarded immediately. Due to the high moisture<br />

content, molds also spread quickly in fruits<br />

and vegetables once they have gained access.<br />

At this stage, mold spores have easy access to<br />

the nutrition they need in order to proliferate.<br />

When in doubt, the entire fruit should be cautiously<br />

discarded, without breaking, squeezing<br />

or damaging it. Such actions would only lead<br />

to further spreading of spores.<br />

Jams or preserves with a sugar content of<br />

more than 50% do not provide a good medium<br />

for molds, since sugar acts as a preservative<br />

at high concentrations. For these products,<br />

it is often sufficient to generously remove mold<br />

spots and the surrounding food. The same approach<br />

applies for hard cheeses that just have<br />

mold on the surface.<br />

To minimize the risk of mold growth,<br />

food should always be stored in<br />

a cool, dry place. <br />

Molds and<br />

mycotoxin research<br />

Since the beginning of time, mankind<br />

has been struggling with molds and<br />

their impact on human life. The earliest<br />

known reference to mold-contaminated<br />

rooms and objects, along with corresponding<br />

recommendations for hygiene,<br />

are found in the Old Testament,<br />

Third Book of Moses (Leviticus). In medieval<br />

times there were regular occurrences<br />

of poisonings, many of them fatal,<br />

following consumption of rye bread<br />

made with flour that contained ergot.<br />

Even in the middle of the 20th century,<br />

thousands of people died after consuming<br />

bread contaminated<br />

with Fusarium mold.<br />

„Mycotoxin Poisoning<br />

has been known for ages -<br />

even over the course of the<br />

Prof.<br />

Manfred<br />

Gareis<br />

last centuries it occurred<br />

quite frequently”, explains<br />

Prof. Manfred Gareis of the<br />

German Federal Agency for<br />

Nutrition and Food, Department<br />

of Microbiology and Toxicology.<br />

However, the triggers for the diseases<br />

and for the symptoms remained in<br />

the dark.<br />

It took massive fatalities among<br />

English turkeys in the 1960’s, and the<br />

associated huge economic loss, to get<br />

science involved in the matter. When<br />

ducks, pheasants and other farm animals<br />

also started perishing from the<br />

mysterious Turkey-X disease, experts<br />

recognized the connection.<br />

Prof. Manfred Gareis: „At that stage,<br />

finally, highly toxic metabolites of Aspergillus<br />

flavus fungi - the aflatoxins were<br />

identified as the cause.” The foundation<br />

for mycotoxin research had been<br />

laid. <br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

21


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

To expose forgeries, the Document Laboratory<br />

of the Zurich Cantonal Police successfully<br />

applies thermal desorption coupled with<br />

GC/MS.<br />

Rolf Hofer, Ph.D.<br />

Forensic Science Division<br />

Head of Document Laboratory<br />

Zurich Cantonal Police<br />

holf@kapo.zh.ch<br />

Andreas Rippert, Ph.D.<br />

Forensic Science Division<br />

Zurich Cantonal Police<br />

ripp@kapo.zh.ch<br />

A new method helps to clearly establish the facts and determine whether<br />

handwritten or printed text is authentic or not. If not, it can be determined at<br />

what point in time the text was altered.<br />

Hot in pursuit of forgers<br />

Forensic science has contributed greatly<br />

to the exposure of forgeries: „Today<br />

we are in a position to determine<br />

if handwritten or printed lines are original<br />

or if they have been manipulated, if documents<br />

have been altered or if they have been<br />

forged entirely”, says Dr. Andreas Rippert<br />

of the Department of Forensic Sciences of<br />

the Zurich Cantonal Police. The forensic<br />

chemist adds: „We can now also pinpoint<br />

the time when a document was forged,<br />

which could help us solve open cases.”<br />

The document laboratory of<br />

the Zurich Cantonal Police<br />

uses a <strong>GERSTEL</strong> Thermal<br />

Desorption System (TDS) in<br />

combination with a <strong>GERSTEL</strong><br />

Cooled Injection System (CIS)<br />

and an Agilent Technologies<br />

GC 6890 / 5973 MSD. The<br />

system is used to differentiate<br />

between ink samples.<br />

Pyrolysis GC/MS<br />

complicates the picture<br />

Pyrolysis GC/MS is often used to examine<br />

paper and documents. The sample is pyrolyzed<br />

under anaerobic conditions, i.e. under<br />

a flow of oxygen-free inert gas. While<br />

Pyrolysis GC/MS provides a lot of information,<br />

the technique does pose a problem, according<br />

to Dr. Rippert: „Attempts to reveal<br />

the document’s material composition using<br />

pyrolysis GC/MS result in a large number<br />

of peaks, which could originate either from<br />

the ink or from the paper. In addition, the<br />

high temperatures used give rise to decomposition<br />

products that further complicate<br />

data interpretation.”<br />

Thermal Desorption – the<br />

method of choice<br />

„To reach a clear conclusion about the authenticity<br />

of a document, a GC introduction<br />

method is needed that provides the<br />

possibility of varying, i.e. programming the<br />

temperature over the course of the thermal<br />

desorption / thermal extraction step. Organic<br />

compounds are extracted from the<br />

sample in successive steps at different temperatures”,<br />

says Dr. Rolf Hofer of the Department<br />

of Forensic Sciences of the Zurich<br />

Cantonal Police. Dr. Hofer and his forensic<br />

expert colleagues used the <strong>GERSTEL</strong> Thermal<br />

Desorption System (TDS) to develop<br />

22<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide Application<br />

“While the complete range<br />

of detected substances<br />

is required for conclusive<br />

classification and<br />

differentiation of written<br />

material, phenoxyethanol<br />

and phenoxyethoxyethanol<br />

are the main indicators<br />

when it comes to age<br />

determination.” Rolf Hofer, Ph.D.<br />

this analysis method. “As carrier gas sweeps<br />

across the paper sample at increasing temperatures,<br />

the relevant analytes ranging<br />

from volatile to semi-volatile, are successively<br />

desorbed and cryofocused prior to<br />

introduction to the GC/MS system.”<br />

Analysis and results<br />

Dr. Andreas Rippert: „At temperatures below<br />

100 °C, volatiles are extracted, especially<br />

phenol and benzene derivatives, as well as<br />

hydrocarbons up to heptadecane.”<br />

At temperatures above 100 °C less volatile<br />

compounds such as fatty acids, phthalates,<br />

and higher-boiling hydrocarbons are<br />

extracted. The scientist explains: “If ink has<br />

been applied to the document during the<br />

past weeks, i.e. in case of „fresh tracks“, hydrocarbons<br />

are emitted in clearly detectable<br />

quantities, as are semi-volatile compounds<br />

like phenoxyethanol and phenoxyethoxyethanol.<br />

At 210 °C, final residues of vola-<br />

World-infamous document forgers<br />

Frank William Abagnale, Jr. became known<br />

as a con-man and check-forger in the late<br />

1960’s and early 1970’s.<br />

After being arrested in 1969 in France,<br />

he was sentenced and sent to prison there.<br />

Subsequently Abagnale was handed over<br />

to the authorities in Sweden, where he<br />

served a further prison sentence. Eventually,<br />

he was extradited to the U.S., and<br />

handed a further 12 year prison sentence.<br />

In 1974, Abagnale was offered an early release<br />

in return for putting his criminal expertise<br />

at the disposal of the U.S. Government.<br />

By applying his knowledge and<br />

experience to legal activities under the<br />

auspices of the FBI, Abagnale has become<br />

one of the leading experts on document<br />

fraud, specializing in check fraud.<br />

tile substances are desorbed even from older<br />

ink samples.” Dr. Rolf Hofer adds: “While<br />

the complete range of detected substances<br />

is required for conclusive classification and<br />

differentiation of written material, phenoxyethanol<br />

and phenoxyethoxyethanol are the<br />

main indicators when it comes to age determination.”<br />

210 C<br />

Residues:<br />

VOC residues from<br />

older text samples.<br />

Catch Me If You<br />

Can: The true<br />

story of a real fake<br />

(Paperback) by<br />

Stan Redding and<br />

Frank W. Abagnale.<br />

He has worked as a consultant for various<br />

banks, airlines, hotels and other companies.<br />

Frank W. Abagnale’s story was documented<br />

by Steven Spielberg in the movie:<br />

“Catch me if you can”, for which Mr. Abagnale<br />

helped write the script. <br />

100 C<br />

During thermal<br />

desorption, the carrier<br />

gas sweeps across<br />

the paper sample at<br />

successively increased<br />

temperatures. During<br />

this process, all relevant<br />

volatile and semi-volatile<br />

compounds are desorbed<br />

and determined.<br />

SVOC:<br />

Long-chain fatty acids,<br />

phthalates, high-boiling<br />

hydrocarbons.<br />

Phenoxyethanol and<br />

phenoxyethoxyethanol<br />

from recently applied inks.<br />

40 C<br />

VOCs:<br />

Phenol- and benzene<br />

derivatives and<br />

hydrocarbons up to<br />

heptadecane.<br />

Using a TDS/CIS-GC/MS system, the document laboratory of the<br />

Zurich Cantonal Police is able to identify ink from ballpoint pens from<br />

different manufacturers. It can also be determined when a particular<br />

text has been written. Cut-outs of less than 5 mm diameter from the<br />

document are sufficient for analysis and conclusive findings.<br />

<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide – May 2007<br />

23


<strong>GERSTEL</strong> <strong>Solutions</strong> Worldwide News<br />

<strong>GERSTEL</strong> Relocation in 2007<br />

<strong>GERSTEL</strong> expands to<br />

accommodate steady growth<br />

Acompany with steady growth is faced<br />

with the challenge of finding room for<br />

the addition of new people and for the expansion<br />

of its manufacturing capacity.<br />

<strong>GERSTEL</strong> has been dealing with this welcome<br />

challenge for most of its 40 year history.<br />

Since 1998, <strong>GERSTEL</strong> has had double<br />

digit annual growth. In 1999, manufacturing<br />

was relocated from company headquarters<br />

to nearby Duisburg, easing the crowded<br />

conditions - at least for a while. Since 2000,<br />

the number of employees has doubled. Adding<br />

to this, the expansion of the products<br />

and services portfolio into the fields of LC<br />

and LC/MS has increased the need for lab-<br />

With increasing market<br />

demand for <strong>GERSTEL</strong>’s<br />

sample preparation solutions<br />

for GC, GC/MS, LC<br />

and LC/MS, growth has accelerated.<br />

Staff has been added<br />

in all departments. After<br />

years of splitting up departments<br />

and remodeling existing<br />

buildings, <strong>GERSTEL</strong> decided that it<br />

was time to build new, modern and efficient<br />

headquarters.<br />

“<strong>GERSTEL</strong> wants to offer customers<br />

maximum performance well into the future,<br />

and this can only be done if our infrastructure<br />

can support further growth”,<br />

states Holger Gerstel. The plan is to relocate<br />

during August and September of 2007. The<br />

decision to stay in Mülheim an der Ruhr<br />

emphasizes the company’s longstanding ties<br />

with the city. The city promptly returned the<br />

favor: As of autumn 2007, <strong>GERSTEL</strong> will reside<br />

at 1 Eberhard Gerstel Platz, the street is<br />

named after Eberhard Gerstel Sr., the company<br />

founder.<br />

Imprint<br />

View of the concrete<br />

shell of the new<br />

<strong>GERSTEL</strong> headquarters.<br />

As of September 2007,<br />

the company will reside<br />

at 1 Eberhard Gerstel<br />

Platz in Mülheim an<br />

der Ruhr.<br />

<strong>GERSTEL</strong> online<br />

You can find more<br />

information on products,<br />

applications and services on<br />

the <strong>GERSTEL</strong> home page at<br />

www.gerstel.com.<br />

Published by<br />

<strong>GERSTEL</strong> GmbH & Co. KG,<br />

Aktienstrasse 232 – 234<br />

45473 Mülheim an der Ruhr, Germany<br />

Eberhard G. (l.) and Holger Gerstel, Owner/Managers<br />

of <strong>GERSTEL</strong><br />

oratory space. “With our LC and LC/MS solutions,<br />

<strong>GERSTEL</strong> has entered into markets<br />

that are developing extremely well for the<br />

company”, say Eberhard G. and Holger Gerstel,<br />

owner/managers of the company.<br />

Since taking over at the helm of the<br />

company in 1998, Eberhard and Holger<br />

Gerstel have steered <strong>GERSTEL</strong> to annual<br />

double digit growth and a world-wide presence<br />

with succesful subsidiaires in the U.S.,<br />

Japan and Switzerland as well as an international<br />

network of distributors spanning<br />

more than 70 countries.<br />

Room for growth – a facility<br />

designed to facilitate the<br />

business process<br />

The new <strong>GERSTEL</strong> headquarters were designed<br />

to support and improve the work<br />

flow and operations at all levels. The facilities<br />

were planned based on extensive employee<br />

consultation.<br />

“In order to have maximum efficiency,<br />

and improve interaction between all departments<br />

and company personnel, we are<br />

bringing three separate locations back together”,<br />

explains Eberhard G. Gerstel.<br />

So this year, only eight years after the relocation<br />

of its manufacturing department,<br />

<strong>GERSTEL</strong> has again reached the point of<br />

having to move. But this time it will be a<br />

happy reunion, that will help secure a successful<br />

future and enable further steady<br />

growth.<br />

Editor<br />

Guido Deußing,<br />

ScienceCommunication,<br />

Neuss, Germany<br />

guido.deussing@t-online.de<br />

Scientific advisory board<br />

Eike Kleine-Benne, Ph.D.<br />

eike_kleine-benne@gerstel.de<br />

Oliver Lerch, Ph.D.<br />

oliver_lerch@gerstel.de<br />

Contact<br />

gerstel@gerstel.com<br />

Design<br />

Paura Design, Hagen, Germany<br />

www.paura.com<br />

Print<br />

BasseDruck, Hagen, Germany<br />

ISSN 1619-0076<br />

G L O B A L A N A L Y T I C A L S O L U T I O N S<br />

<strong>GERSTEL</strong> GmbH & Co. KG<br />

Aktienstraße 232 - 234<br />

45473 Mülheim an der Ruhr<br />

GERMANY<br />

+49 208 - 7 65 03-0<br />

+49 208 - 7 65 03 33<br />

gerstel@gerstel.de<br />

www.gerstel.de<br />

<strong>GERSTEL</strong>, Inc.<br />

1510 Caton Center Drive<br />

Suite H<br />

Baltimore, MD 21227<br />

USA<br />

+1 410 - 247 5885<br />

+1 410 - 247 5887<br />

info@gerstelus.com<br />

www.gerstelus.com<br />

<strong>GERSTEL</strong> AG<br />

Enterprise<br />

Surentalstrasse 10<br />

6210 Sursee<br />

SWITZERLAND<br />

+41 41 - 9 21 97 23<br />

+41 41 - 9 21 97 25<br />

gerstel@ch.gerstel.com<br />

www.gerstel.de<br />

<strong>GERSTEL</strong> K.K.<br />

2-13-18 Nakane<br />

Meguro-ku<br />

152-0031 Tokyo<br />

JAPAN<br />

+81 3 57 31 53 21<br />

+81 3 57 31 53 22<br />

info@gerstel.co.jp<br />

www.gerstel.co.jp<br />

Subject to change.<br />

<strong>GERSTEL</strong>, GRAPHPACK and<br />

TWISTER are registered trademarks of<br />

<strong>GERSTEL</strong> GmbH & Co. KG.<br />

Printed in Germany · 0407b<br />

© Copyright by <strong>GERSTEL</strong> GmbH & Co.KG

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