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