hot, hotter, bombfire the new nexera mikros pop the corks · flavors in beer determined by...
TRANSCRIPT
Hot, Hotter, Bombfire
Pungency of Currywurst
The new Nexera Mikros
New micro-flow LC-MS solution –high sensitivity, durability and ease-of-use
Pop the corks:
50th anniversary of Shimadzu in Europe
Pharmaceutical
Plastics and Rubber
CONTENT
Clinical
Chemical, Petrochemical,Biofuel and Energy
How X-ray fluorescence can supportconsumer prices stability –All-in-one analysis with EDX-8000P 2
Into the microwave! – Analysis offatty acids in foods 4
New solutions for treating plasticwaste – FTIR analysis of biodegrad -able polymers from everyday life 6
Hot, Hotter, Bombfire – Pungency of Currywurst 10
Olive oil is top source of vitamin E – A quantitative fluorescence analysis of tocopherols 12
Flavors in beer determined byHeadspace-GC – GC-2010 Plus in the Quality Control procedure of a large Greek brewery 14
APPLICATION
Troubleshooting via YouTube – Video tutorials using the new GC generation Nexis GC-2030 as an example 18
Pop the corks: 50th anniversaryof Shimadzu in Europe – Time tocelebrate 20
LATEST NEWS
Guardian in the chemical park – TOC process measurement at Leuna Chemical Park, Germany 16
Less than a teaspoon of blood can predict Alzheimer’s disease risk 19
READ FOR YOU
MARKETS
New micro-flow LC-MS solution –Nexera Mikros provides high sensi-tivity, durability and ease-of-use 9
PRODUCTS
SHIMADZU NEWS 1/2018
Food, Beverages, Agriculture
Environment
Automotive
How X-ray fluorescencecan support consumerprices stabilityAluminum fluoride all-in-one analysis with EDX-8000P
N owadays, aluminum as achemical element plays animportant role in every-
day life. Due to its low weightand good thermal conduction,aluminum and its alloys are thebasis for modern aviation indus-try, aerospace engineering, pro-duction of automobiles, rollingstock for high speed trains, seaand river vessels...
Moreover, this element is ex -tremely popular in the produc-tion of cookware or foils usedfor packaging in the food indus-try.
Aluminum is produced by elec-trolysis of alumina dissolved in a molten cryolite bath. The pro -
cess of electrolysis requires ahuge amount of electricity. Someindustrial processes using alu-minum fluoride AlF3 (approxi-mately 5 - 15 %) and other addi-tives have been developed todecrease the melting point to 930- 950 °C and to increase conduc-tivity of the electrolyte solution.This reduces energy consump-tion and greatly decreases thecost of the aluminum.
Before being used as an additive,aluminum fluoride has to be ana-lyzed in order to check the con-tent of the main component. Atthe same time, the main impurity(aluminum oxide) as well asharmful elements such as silicon,phosphorus and iron are exam-
ined in order to prevent mainproduct contamination (metallicaluminum).
AlF3 quality analysis: a constant challenge for laboratories
According to the Russian GOSTregulation (national standard ofthe Russian Federation and CIScountries), standard chemicalanalysis of aluminum fluorideincludes many time-consumingsample preparation steps includ-ing fusion and dissolution. Inaddition, different analysis meth-ods are used for each compound:titration for quantitative analysisof AlF3, free aluminum oxide(Al2O3) determination by trilo -
Figure 1: Aluminum cookware: the easiest way to cook and transport various
food dishes
EDX
0.12
0.021
0.027
EDX
0.14
0.027
0.01
Chem.
0.16
0.026
< 0.02
EDX
0.16
0.024
0.015
SiO2
P2O5
Fe2O5
Russian Standard
GOST 19181-78
> 0.25
> 0.05
> 0.08
Sample 1 Sample 2 Sample 3 Sample 4
Chem.
0.15
0.026
< 0.02
EDX
0.18
0.025
0.015
Chem.
0.11
0.03
< 0.02
Chem.
0.09
0.018
0.030
Concentration, wt. %
EDX
95.9
2.2
EDX
96.0
2.1
Chem.
95.8
2.5
EDX
95.2
2.3
AIF3AI2O3
Russian Standard
GOST 19181-78
> 93
> 4
Sample 1 Sample 2 Sample 3 Sample 4
Chem.
94.5
2.7
EDX
94.9
2.6
Chem.
96.1
1.9
Chem.
96.0
2.1
Concentration, wt. %
APPLICATION
3SHIMADZU NEWS 1/2018
Table 1: Comparison of results of main component and Al203 in AlF3 analysis by chemical methods (Chem.) and EDX-8000P
Table 2: Comparison of results for SiO2, P2O5 and Fe2O3 analysis by chemical methods (Chem.) and EDX-8000P
0.0 0.00 0.0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
0.02
0.03
0.06
0.08
0.10
0.12
0.14
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0Si K� P K� Fe K�
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 0.000 0.005 0.010 0.015 0.020 0.025 0.030 0.035 0.000 0.005 0.010 0.015 0.020
Figure 3: Calibration curves obtained for each targeted contaminant
nometric measurement of alu-minum, and photometric analysisof silicon, phosphorus and ironoxides (SiO2, Fe2O3 and P2O5).So, complete analysis of one sam-ple (including sample preparation)takes more than twelve hours andrequires many chemical reagentsand devices.
Use of the EDX-8000P EnergyDispersive X-ray fluorescencespectrometer appears to offer avaluable alternative way to simpli-fy and dramatically decrease ana -lysis time. This spectrometer is infact able to analyze all elementsfrom carbon up to uranium in asimultaneous measurement. More -over, target concentration rangesare compatible with the EDXspectrometer sensitivity. TheEDX-8000P is BfS (safety stan-dards of the German FederalInstitute for Radiation Safety)type approval certified.
New fast and easy X-ray fluorescence method for AlF3 analysis
Samples of AlF3 were preparedfor analysis by grinding in themixer mill and pressing in the pel-let press. The same sample prepa-ration is used for single AlF3 stan-dard sample with a known contentof the main component andAl2O3. Calibration samples foranalysis of SiO2, P2O5 and Fe2O3were prepared by adding knownamounts of element oxides toAlF3 standard sample and subse-quent mixing, grinding and press-ing.
A routine measurement procedureof unknown sample by Funda men -tal Parameters (FP) method is in -
cluded in the standard spectrome-ter software (PCEDX). Neverthe -less, a single standard sample wasused to perform methods calibra-tion in order to improve accuracyof results. Aluminum fluoridecontent was calculated on thebasis of fluorine element concen-tration. Aluminum oxide Al2O3concentration was then evaluatedby the aluminum peak after alu-minum fluoride subtraction.Results of X-ray and chemical
(titration and photometry) analy-sis obtained for fluorine and alu-minum are given in table 1.
The other contaminants (silicon,phosphorus and iron oxides) wereanalyzed using calibration curvemethod with corresponding ele-ment specific K� lines. Calibra -tion curves for each oxide areshown in figure 3. The results ofX-ray and chemical analyses aregiven in table 2.
Total analysis time of all elementsincluding sample preparation wasonly approximately thirty minu -tes.
Conclusion
All EDX results shown in tables 1and 2 showed excellent correlationwith official regulation analysismethods results. This demon-strates that the EDX-8000P analy-sis procedure is a valuable alterna-tive to traditional time-consumingmethods. By decreasing analysistime and chemical product con-sumption, this new strategy cancontribute to reduced aluminummaterial prices and in the end toprice stability of consumer pricesfor food packaging, conveniencefoods and freshly prepared mealson wheels.
Acknowledgements
We gratefully acknowledge thevaluable advice and assistance inEDX analysis of our colleaguesfrom the accredited Analit Com -pany (St. Petersburg, Russia) labo-ratory.Figure 2: Energy dispersive X-ray fluorescence spectrometer EDX-8000P
T he EU regulation on theprovision of food informa-tion to consumers (No.
1169/2011) [1] requires all foodmanufacturers to label their prod-ucts with information on the con-tent of saturated and unsaturatedfatty acids. The new regulationaims to provide more transparen-cy to consumers so that they havea sound basis for making a deci-sion on whether or not to buy aproduct.
Analysis of fatty acids is based ondetermination of the total fat con-tent using the Weibull-Stoldtmethod (ISO 8262-1 [2]), fol-lowed by derivatization of thefatty acids to volatile fatty acid
ous digestion and extraction of thelipids. The microwave used forthis was a Discover SP-D® instru-ment manufactured by theGerman-based CEM company.
Total fat contents of the referencematerials investigated – milk pow-der and chocolate – were recov-ered completely. All non-certifiedsamples also gave very good recov -ery rates of > 90 wt.-% total fatwith standard deviations between0.6 and 3.7 wt.-%. This clearlydemonstrates that successfuldetermination of the total fat inreal samples using the microwavemethod is matrix-dependent.
In particular, the homogeneity ofthe sample influences the com-pleteness of the extraction. Thisespecially affects foods such aspotato chips and infant formulapowder due to their inhomogene-ity or to the complexity of theircomposition. The recovery rate ofthese samples can be increased byapprox. 15 % by means of repeat-
methyl esters (FAMEs) accordingto ISO 12966-2:2011, and theirGC analysis according to ISO12966-4:2015 [3]. The ISO stan-dards form the basis of a newmethod recently developed at theUniversity of Applied Sciences in Krefeld, Germany that usesmicrowave-assisted extraction andanalysis of saturated and unsatu-rated fatty acids. This method hasalready been presented in thejournal Chromatography Today5-6/16.
Whereas the ISO method deter-mines total fat by means of diges-tion in hydrochloric acid followedby Soxhlet extraction, the micro -wave method involves simultane-
APPLICATION
4 SHIMADZU NEWS 1/2018
Into the microwave!Analysis of fatty acids in foods
ed extraction (cold). These stepsare carried out with fresh solventafter digestion. As a compromisebetween complete recovery andrequired analysis time and con-sumption of chemicals, threeextraction steps were carried outfor each analysis.
ISO vs. microwave
In the long term, the microwavemethod of determining total fatpresents an attractive alternativebecause it offers considerable sav-ings in resources. Experimentsshowed that a single determinationof total fat using the micro wavemethod takes 1.5 h, whereas theISO method takes up to 9.5 h. Themicrowave method thus of fers atime saving of 8h while also requir -ing less instrumentation. Further -more, it requires much smallerquantities of chemicals, particular-ly organic solvents (figure 3).
The actual analysis of fatty acidsis carried out using gas chroma -
Recovery rate [wt.-%
]
100.0
120.0
60.0
80.0
20.0
0.0
40.0
Whole milk3.5 %
94.3 90.7 92.5100.4 99.7 97.5
Fish19.1 %
Formula24.2 %
Milk powder26.67 %
Chocolate32.2 %
Potato chips33.8 %
Figure 1: Recovery rates of the total fat contents of all food samples investigated; the milk
powder and chocolate are certified reference materials. For the other samples, a reference
value was determined with the ISO method.
Figure 2: Plot of the fat extracted per extraction and increasing recovery rates (RR)
for the extraction of a salmon sample using the microwave method
Recovery rate [wt.-%
]
100.0
110.0
120.0
80.0
90.0
60.0
50.0
70.0
100
120
140
60
80
20
00 1 2 3 4 5 6
40 m (fats) [m
g]
Number of extractions
Injection volume
Injector temperature
Split ratio
Column type
Column length
Inner diameter
Film thickness
Detector
Detector temperature
Mobile phase
Carrier gas flow
Injector
1 µL
250 °C
1:100
FAME WAX
30 m
0.25 mm
0.25 µm
FID
250 °C
Helium
35 cm/s
SPL (Split)
Table 1: Parameters for GC analysis of the FAMEs using a GC-2010 Plus instrument
Min.
uV
050,000
100,000150,000200,000250,000 ISO
7.5 10.0 12.5 15.0 20.0
Min.
uV
050,000
100,000150,000200,000250,000
7.5 10.0 12.5 15.0 20.0 22.5 25.0
17.5 22.5 25.0
17.5
Micro
5SHIMADZU NEWS 1/2018
APPLICATION
tography. With respect to requiredtime and consumption of chemi-cals, the new microwave derivati-zation is very similar to the gener-al methods described in ISO12966-4. An alkali- and an acid-catalyzed derivatization step areeach carried out to convert bothbound and free fatty acids toFAMEs. Parameters used for GCanalysis of the FAMEs with aGC-2010 Plus from Shimadzu aresummarised in table 1.
The 37-component FAME mixfrom Supelco company was usedfor identification. The GC method
applied was able to separate allFAMEs present, except for thecis/trans isomers of oleic acid(C18:1). Figure 4 shows the chro-matogram of the FAMEs presentin a sample of infant formulapowder.
The peak areas have a linear rela-tionship with the mass fractionsso that summation over the peakareas enables determination of thepercentage fractions of the satu-rated and unsaturated fatty acids.The microwave method for theinfant formula powder (chroma -togram) gives a fraction of 41.6 ±
0.12 wt.-% for saturated fattyacids and 58.4 ± 0.12 wt.-% forunsaturated. Figure 5 comparesthe percentage mass fractions ofthree samples obtained using theISO and the microwave methods.
This shows that the mass fractionsof saturated and unsaturated fattyacids obtained with the two meth-ods are in agreement, and themicrowave method is thus qualita-tively equivalent to the ISOmethod. This also applies to thesample of potato chips, whichcontained an enormously highfraction of unsaturated fatty acids.
Some samples, e.g. salmon, gaveslight deviations in the ratio ofsaturated to unsaturated fattyacids. A closer look at the chro-matograms of the salmon samplereveals slight differences for bothmethods. For example, fatty acidsC21:0 and C22:6 were not foundusing the microwave method, incontrast to the ISO method. Fur -ther investigations are necessary inthis context.
Conclusion
GC-FID is a simple way of deter-mining saturated and unsaturatedfatty acids in foods. For samplepreparation, the microwavemethod of extracting fatty acids infoods can be used as the basis foranalyzing a wide range of foodsamples. Compared to conven-tional ISO methods, it savesresources with respect to bothchemicals and time and also givescomparable results.
AuthorsAurelia Bertini, Jürgen Schram 1
Frank Scholten, Ulf Sengutta 2
Franz Kramp, Uwe Oppermann 3
1 Hochschule Niederrhein
Frankenring 20, D-47798 Krefeld
Germany2 CEM GmbH
Carl-Friedrich-Gauß-Strasse 9
D-47475 Kamp-Lintfort
Germany3 Shimadzu Europa GmbH
Albert-Hahn-Strasse 6 -10
D-47269 Duisburg
Germany
Literature[1] The European Parliament and Council of
the European Union, “Regulation No.
1169/2011 of the European Parliament
and of the Council,” No. 1169. pp. 18-63,
2011.
[2] Deutsches Institut für Normung e.V.,
“Bestimmung des Gesamtfettgehalts in
Fleisch und Fleischerzeugnissen-
Gravimetrisches Verfahren nach Weibull-
Stoldt” (Determination of the total fat
content in meat and meat products –
Gravimetric determination using the
Weibull-Stoldt method). Beuth Verlag
Berlin, 2014.
[3] Deutsches Institut für Normung e.V.,
“Animal and vegetable fats and oils –
Gas chromatography of fatty acid methyl
esters – Part 4: Determination by capil-
lary gas chromatography (ISO 12966-
4:2015)”. Beuth Verlag Berlin, 2015.
Figure 6: Top chromatogram: Analysis of salmon using the ISO method. Bottom chromato-
gram: Analysis of salmon using the microwave method.
Figure 3: Required time and consumption of chemicals for a single total fat determination
using the microwave and ISO methods
Figure 4: Chromatogram of the FAMEs from infant formula powder using the
microwave method
Time [m
in]
Chemical con
sumption [m
L]
0
100
200
300
400
500
600
ISO Microwave
10
180
375102054 0
200
400
600
800
1,000
1,200
ISO Microwave
100
300
600 3.5207.5
Minutes
uV
050,000
100,000150,000200,000250,000300,000350,000400,000450,000
2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5
Recovery rate [wt.-%
]
100.0
120.0
60.0
80.0
20.0
0.0
40.090.9%
9.1%
91.3%
8.7%
58.6%
41.4%
58.4%
41.6%
72.3%
27.7%
69.9%
30.1%
FormulaISO
FormulaMicro
SalmonISO
SalmonMicro
Potato chipsISO
Potato chipsMicro
Figure 5: Fractions of saturated and unsaturated fatty acids in potato chips, infant formula
powder and salmon determined with the microwave and ISO methods
APPLICATION
6 SHIMADZU NEWS 1/2018
E very year, an estimated 140million tonnes of plastic areproduced from fossil fuels
[1]. Much of this is intended forthe production of consumer goodssuch as food packaging or dispos-able tableware. But what happensto plastic after it has been dis-posed of?
Recycling large proportions of theplastic requires much effort. Aftera few cycles, however, it becomesplastic waste and ends up in land-
fills. From there, it makes its wayinto the environment as micro -plastic [2]. The microplastic thenbecomes part of the food chain,and returns sooner or later to theconsumer.
In 2014 on the Dutch island ofTexel, the stomach contents of fulmars were tested for polymers,a scientific project driven by Dr. J. A. van Franeker, Wagenin -gen University & Research. Onaverage, about 0.3 g of plastic per
New solutions for treating plastic wasteFTIR analysis of biodegradable polymers from everyday life
bird (700 g) stomach was found;compared to a human with 70 kg,this is equivalent of the capacityof a lunch box filled with plastic[3]. This illustrates the problem of
microplastics in the environment.For many years, research has ad -dressed the situation. The solutionto the problem is called biodegrad-able plastics.
Figure 1: Chemical Structure of Polylactic Acid (PLA)
0
1
4,000 3,500 3,000 2,500 2,000 1,750 1,500 1,250 1,000 750 500cm-1Spoon, colored, white, one way spoon (biodore)
Abs
0
1
4,000 3,500 3,000 2,500 2,000 1,750 1,500 1,250 1,000 750 500cm-1Poly(lactide-co-glycolide), ca. 48 wt. % oxylactoyl units
Abs
0
1
4,000 3,500 3,000 2,500 2,000 1,750 1,500 1,250 1,000 750cm-1Poly(lactide-co-glycolide), ca. 48 wt. % oxylactoyl units
Abs
0
1
4,000 3,500 3,000 2,500 2,000 1,750 1,500 1,250 1,000 750cm-1TALC(Polyethylene, Chlorosulfonated) DuraSampl IR-II
Abs
APPLICATION
7SHIMADZU NEWS 1/2018
Biodegradable plastics in food packaging
Analysis of food packaging revealstraces of biodegradable plastics.So far, about 200 plastic packagingof foodstuffs have been analyzedfor their main components usinginfrared spectroscopy (FTIR). Thiswas done with the IR-Tracer100FTIR spectrophotometer in com-bination with an ATR (attenuatedtotal reflection) diamond reflec-tion unit. Five of the samples test-ed are labelled as “biodegradable”,more specifically: two teabags,one garbage bag, disposable cut-lery and the lid of a disposablecoffee cup (figure 2). The sampleswere from England, Germany andthe Netherlands.
Figure 3 shows that the ATRspectrum of the disposable spoonhas similarities to the spectrum ofmodified polylactic acid (PLA).The additional peaks at 1,010 cm-1
and 667 cm-1 are due to the stretch -ing and deformation vibrations ofthe Si-O bond, suggesting thepresence of talc as a filler [4].
Which polymers are in disposable dishes?
PLA is a polymer consisting oflactic acid monomers that can beproduced by lactic acid bacteria.Biodegradation is carried out bymicroorganisms, or rather throughtheir excreted enzymes (esterases,proteases, lipases). In the simulat-ed composting of a PLA bottle, itwas found that it took about sixweeks until over 80 % of the bot-tle was broken down into CO2and water [1]. PLA is therefore adesirable alternative to plasticssuch as PP, PE or PS.
A big disadvantage of PLA, how-ever, is its high brittleness. Thedisposable spoon, for example, isvery rigid and breaks easily,strongly limiting applications ofthe biological plastic as a packag-ing material. To circumvent thisdifficulty, attempts have beenmade to add low-molecular plasti-cizers to PLA [1]. Other disad-vantages are the low heat resist-ance and higher production costs.
In addition to packaging materials,3D printing and medical technolo-
gy are other possible fields of ap -plication for PLA. Medical tech-nology benefits above all from thedegradation properties of PLA.Implants made of PLA (e.g.screws) can be designed so thatthey are absorbed by the bodyover a defined period of time.Other applications in the medicalfield include sutures and micros-pheres for the release of activeingredients [5].
Biodegradable polymers in a tea bag
Analysis of the biodegradable teabags showed that both are alsomade of PLA. This polymer re -places the commonly used PET(polyethylene terephthalate). Ear -lier research has shown that PETteabags contain about 200 ppm ofantimony, leading to significantcontamination of the tea duringthe brewing process [6]. Due tothe harmful properties of �
Figure 2: Analyzed samples consisting of biodegradable polymers (declaration on the products)
Figure 3: IR spectrum of plastic spoon (a), IR database spectrum of modified PLA (b),
differential spectrum of a and b (c), IR database spectrum of talc (d)
0.175
0.150
0.125
0.100
0.075
0.050
0.025
0.000
0.200Abs
PLA
4,400 4,000 3,600 3,200 2,800 2,400 2,000 1,800 1,600 1,400 1,200 1,000 800 600 400
Tea bag, outside, chocolate cha cm-1
0.250
0.225
0.200
0.175
0.150
0.125
0.100
0.075
0.050
0.025
0.000
0.275Abs
PET
4,400 4,000 3,600 3,200 2,800 2,400 2,000 1,800 1,600 1,400 1,200 1,000 800 600 400
Bag, transparent, inside, herbal tea-Kräutertee Cool Mint cm-1
APPLICATION
8 SHIMADZU NEWS 1/2018
Figure 5: Comparison of spectra of PLA teabag with a conventional PET teabag
antimony, the use of PET in tea -bags may present a health risk.EDX (energy-dispersive X-rayfluorescence) analysis of the PLAtea bags shows that neither anti-mony nor other harmful heavymetals are detectable here. Thismakes PLA more environmentallyfriendly, and also safer as a mate-rial for tea bags.
PBT in garbage bags
Finally, the “biodegradable” gar -bage bag should be mentioned.FTIR analysis confirms that this isnot PLA but polybutylene tereph-thalate (PBT). There is also evi-dence of glycogen in the IR spec-trum, a widely branched polysac-charide that acts as a storagemedium in the human body. It ismade up of numerous glucoseunits and, in the case of the gar -
bage bag, connects the PBT chains[7]. At the same time, it offers apoint of attack for breaking downof the chains by chemical or bio-logical hydrolysis. Unlike PLAwhich can be broken down micro-bially to water and CO2, thedecomposition here is really areduction of chain length.
Summary
PLA bioplastic is a popular alter-native to fossil-based polymers. It is already being used in a wide
variety of applications but has notyet prevailed over conventionalplastics in the food packaging sec-tor. In addition to cost reasons,this is mainly due to inadequatematerial properties. ATR analysisof the samples presented showsthat FTIR spectroscopy is a suit-able method to identify biode -gradable polymers and their addi-tives non-destructively in a mini-mal amount of time. Additionally,with the EDX technique, it is pos-sible to easily determine the ele-mental composition of the poly-mer and to assess the safety of theproduct.
Literature[1] Madhavan Nampoothiri K., Rajendran
Nair N., Pappy John R.,
An overview of the recent developments
in polylactide (PLA) research, NIIST,
India, 2010.
[2] Amass W., Amass A., Tighe B.,
A Review of Biodegradable Polymers:
Uses, Current Developments in the
Synthesis and Characterization of
Biodegradable Polyesters, Blends of
Biodegradable Polymers and Recent
Advances in Biodegradation Studies,
POLYMER INTERNATIONAL, 1998,
VOL. 47, NO. 2.
[3] Van Franeker, J. A.,
Fulmar Litter EcoQO monitoring in the
Netherlands – Update 2014. IMARES
Report C123/15. IMARES, Texel. 55 pp.,
2015.
[4] Farmer V. C.,
The infrared spectra of talc, saponite
and hectorite, The Macaulay Institute
for Soil Research, Aberdeen, Scotland,
1958.
[5] Ruffieux K., Wintermantel E.,
Resorbierbare Implantate.
In: Medizintechnik Life Science Enginee -
ring, Springer, Berlin, Heidelberg, 2008.
[6] Egelkraut-Holtus M., Knoop J., Ortlieb M.,
Antimony in Breakfast Tea?
Consequences Going Hand in Hand with
Today’s Materials, G.I.T. Laboratory
Journal 1-2/2015, 26-27.
[7] www.chemie.de/lexikon/Glykogen.html
[cps/uA]
0.00
0.25
0.50
0.75
1.00
10.00 20.00 30.00[keV]
Figure 4: EDX spectrum of a PLA teabag (excitation energy 50 kV). Neither antimony nor
other harmful heavy metals have been detected.
PRODUCTS
9SHIMADZU NEWS 1/2018
Nexera Mikros provides high sensitivity, durability and ease-of-use
New micro-flow LC-MS solution
T he Nexera Mikros is abrand-new LC-MS accom-modating a wide range of
flowrates, from semi-micro flow -rates (100 to 500 µL/min) whichare often used for analysis inexisting systems, to micro flow -rates (1 to 10 µL/min). This sys-tem achieves both durability andoperability while enabling analysiswith a significant increase in sen-sitivity.
Nexera Mikros complements theNexera series, featuring NexeraX2, XR, MP, Nexera-i and NexeraUC systems to maximize analyti-cal productivity. The Nexeraseries is a unique approach todelivering high-quality, high-speed LC-MS analysis combiningthe Nexera UHPLC and anyShimadzu single or triple quadru-pole UFMS solution as a seam-lessly integrated system.
With Nexera Mikros, Shimadzucontributes to improving produc-tivity at pharmaceutical companiesand clinical contract researchorganizations. The new LC-MSsets a new standard in instrumentoperability, processing speed andease-of-use as well as samplethroughput.
Ten times more sensitivity
Compared to existing LC-MS systems, Nexera Mikros providesat least ten times more sensitivity.This is achieved by the LC-Mikros,a solvent delivery pump with anew control system, reducing pul-sation while delivering a stablesolvent flow even at low microflowrates. In addition, positioningof the ionization interface hasbeen optimized for more efficient
sample introduction into the massspectrometer.
UF-Link achieves both high-sensitivity analysis andimproved operability
Microscopic gaps (dead volume)in the piping connectors lead to adecrease in sensitivity by causingpeak dispersion. UF-Link, a con-nection mechanism betweenShimadzu’s newly developed ana-
Nexera Mikros
lytical column and the mass spec-trometer, ensures high sensitivityand, at the same time, enablesone-touch connection between theanalytical column and the ioniza-tion interface for the mass spec-trometer. In addition, UF-Link iscompatible with connectionsbetween commonly used analyti-cal columns and the ionizationinterface, so column selection isflexible to suit the target sample.
Higher efficiency of investments in R&D
The LC-Mikros solvent pumpdelivers a wide flowrate range,from micro flowrates of 1 µL/minto semi-micro flowrates of 500 µL/min. By enabling analysis compa-rable to existing LC-MS systems,and high-sensitivity analysis atmicro flowrates, this single unitimproves the operational efficien-cy of the LC-MS system andshortens research and develop-ment times.
NEWS *** LATEST NEWS *** LATEST NEWS *** LATEST NEWS *** LATEST NE
1/3 less large and twice as fast New Nexgen GC CAGC-100 – Compared with conventional technology,more than 30 % smaller and up to 50 % less analysis time / compactAnalyzer Gas Chromatograph “Nexgen GC” / Plate column and multi-deans switch proprietary technologies
Celebrating thisyear the 50th an -ni versary of itspresence in Eu -rope, Shimadzuemphasizes itsExcellence in
Science approach through therelease of the new next-genera-tion “Nexgen GC” multidimen-sional gas chromatograph. TheNexgen GC highlights the com-pany’s position of a world leaderin analytical instrumentation. It achieves miniaturization andhigh-speed analysis by the pro-prietary “plate column” technolo-gy and multi-deans switch (pat -ented technology). It is a nextgeneration GC making it easy touse multidimensional analysissuitable for complex componentsby installing two gas chromato -graphs in a small body.
Improved analytical productivity
The conventional multidimension-al gas chromatograph (MDGC)uses two ovens equipped withcapillary columns, therefore thesystem becomes large and diffi-cult to install. Analysis also takestime, so there may be issues interms of suitability for processingin areas such as quality control. The Nexgen GC was developedto solve these problems. It re -quires of about 1/3 less laborato-
high-speed and high separationanalysis is possible. In addi-tion, analysis time can beshortened by “backflush func-
ry space compared to conven-tional models, and can raise thechromatographic speed fasterthan before, so it is possible tohalve the anal ysis time [1]. Fur -thermore, it im proves analyticalproductivity through high speedand space saving.
The Nexgen GC is equippedwith new and advanced productfeatures such as:
1. Built-in two plate columns in a compact bodyThe newly developed platecolumn is a compact, high per-formance GC column whichforms a fine flow path by pho -to etching [2] on a 100 mm x100 mm plate. This product isan MDGC configuration withtwo column cartridges built ina compact body.
2. High-speed and high separation analysis possibleSince the column is heateddirectly by the flat plate heaterarranged inside the cartridge, it can raise the temperature by70 °C per minute from the lowtemperature range (near roomtemperature) to the high tem-perature range (350 °C), whichwas not possible with the con-ventional oven type GC [3[.Since each of the two car-tridges can be heated quickly,
tion” which drives out notquantified high boiling pointcompounds remaining after elu -tion of the target component. �
1/3 less large and twice as fast: The “Nexgen GC”Compact Analyzer Gas Chromato -
graph improves analytical productivity through high speed while saving space
SHIMADZU NEWS 1/2018
SHIMADZU NEWS 1/2018
3. Heart cut with high repeatabilityIn the Shimadzu “heart cutanalysis” [4] which introducesonly the target component inthe sample for improved sepa-ration to a second column, thecompany’s proprietary “multi-deans switch” has been adopt-ed. Hardly any pressure changeoccurs at the first dimensioncolumn outlet, variation of re -tention time is suppressed and
high repeatability is achievedthat can perform heart cut morethan once.
4. High operabilityA full color liquid crystal touchpanel enables easy operation.Various functions such as self-diagnosis, automatic leak checkof carrier gas, display of chro-matogram etc. are possible withthe GC body. An advanced userinterface can analyse the state
of the device at a glance anddisplay the parameter settingscreen with one click in theuser-friendly “LabSolutions”software. Remote monitoring ofthe device is also possible usinga smartphone or tablet PC.
[1] Analysis time that can be abbreviated
depending on the subject of analysis
[2] Precision processing technology for
forming of a corrosion-resistant film on
a glass or metal plate with a necessary
pattern using photolithography techno-
logy
[3] The conventional product can raise the
temperature range from 250 to 350 °C at
45 °C / min, Nexis GC-2030. 230V models
[4] Technology to introduce components
that cannot be separated by one column
into the second column by switching the
switching mechanism
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SHIMADZU NEWS 1/2018
The new UV-1900UV-Vis spectropho-tometer is equippedwith an ultrafastscan function thatenables data acquisi-tion of 29,000 nm/
min (it takes about three secondsto measure in visible region), thefastest level in the industry. It’soutstanding features representShimadzu’s value proposition of“Excellence in Science”.
The UV-1900 features a large,easy-to-use color touch panel aswell as excellent operability. Allfunctions are directly reachablewith large and easy to understandicons. In addition, UV-1900 pat -ented LOW-RAY-LIGH® diffrac-tion grating technology ensureslow stray light with high resolu-tion and one of the largest rangesof linearity.
While UV-1900 can be operated asa standalone instrument the newLabSolutions UV-Vis (Shimadzu’sUV-Vis control software releasedsimultaneously) expands user pos-sibilities. This software also con-tributes to data pass/fail judg-ments via its spectral evaluationfunctions.
UV-1900 can connect withShimadzu’s analysis data manage-ment systems (LabSolutions DB/CS) in order to provide fully inte-
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By detecting ultraviolet and visi-ble light passed through or reflect-ed by samples, UV-Vis spectro -
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Industry’s fastest level scan function and LabSolutionsUV-Vis control softwareNew UV-1900 UV-Vis Spectrophotometer – High-accuracy quantitativeanalysis in regulated environments / proven excellent spectroscopic capabilities from high-end models / compliant with the pharmacopeia of various countries incl. FDA 21 CFR Part 11
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popular, and demand for UV-Visspectrophotometers continues toexpand, even in newly emergingeconomies. Accordingly, whenusers select an instrument, theyfocus on cost effectiveness, oper-ability, compliance with variousnational regulations and en hancedmanagement functions.
Against this background, the UV-1900 was developed fordeployment in an even widerrange of regions, including Cen -tral and South America. Shimadzuis deploying the UV-1900 world-wide, making the most of thecombination with LabSolutionsUV-Vis, a control software idealfor quality control and integratedmanagement with other models.Special features of the UV-1900UV-VIS-NIR Spectrophotometerare:
1. High performance matched to a variety of sample analysesA newly developed ultrafastscan function enables dataacquisition as fast as 29,000 nm/min. By performing repeatmeasurements, the process ofsample changes in chemicalreactions can be analyzed in a
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10 SHIMADZU NEWS 1/2018
Pungency of Currywurst
E very culture has its ownfamous fast food dish orstreet food, to use a current
buzzword. The UK is famous forits fish and chips, Denmark for itshot dogs, The Netherlands for Fri -kandel, and Germany for its friedpork sausage with curry sauce, theso-called Currywurst. AlthoughBerlin claims to have invented thisdish, the Ruhr area with 5 millionpeople in the west of the countryhas the highest density of fast foodrestaurants offering Currywurstseasoned with curry ketchup, asauce based on spiced ketchup or tomato paste. The dish oftencomes with French fries.
Over 800 million curry sausagesare consumed annually in Ger -many [1], some with hot or veryhot sauces added. According toowners of “Die Currywurst”,their Ruhr area-based snack barprovides the world’s hottest Cur -rywurst. Shimadzu has received
some samples for analysis, includ-ing the hottest sauce. Guests eatthem at their own risk, and theyare served with the warning: “maythreaten health”.
The pungency (hotness) of a prod -uct is measured in Scoville HeatUnits (SHU). Tabasco has a pun-gency of 2,500 to 5,000 Scoville,while the “Bombfire” sauce, owncreation of the “Die Currywurst”snack bar, has up to 666,000 Sco -ville.
Pungency level determinationwith HPLC
Pungency of the various saucesdepends on the amount of capsai-cinoids which are naturally pres-ent in bell peppers or chili pep-pers. The two main components,capsaicin (69 %) and dihydrocap-saicin (22 %), are almost twice asstrong as the capsaicinoids nordi-hydrocapsaicin (7%), homodihy-
drocapsaicin (1%) and homocap-saicin (1%), which are smaller incomparison. Therefore, only cap-saicin and dihydrocapsaicin arestudied to determine capsaicin lev-els in the various sauces and purechili peppers [2].
To measure the exact content, thei-Series LC-2040C 3D compactHPLC system was used for high-speed analysis. Equipped with aphotodiode array (PDA) and fluo-rescence detector, standards of thetwo main components were ana-lyzed first. The method parame-ters applied are based on an exist-
ing Shimadzu application (No.L335) and are listed in table 1.
First, capsaicin and dihdrocap-saicin standards are tested in dif-ferent concentrations (5, 10, 25,50, 75 and 100 µg/mL) to create acalibration curve. Fluorescencedetection exhibits approximately16-fold higher sensitivity thandetection with the PDA, as shownin figure 1.
Focus will therefore only be onthe fluorescence detector analyses.The assignment of the two peaksis shown in figure 2, where the
Figure 2: RF chromatogram of the standard 5 µg/mL
Hot, Hotter, Bombfire
0
1,000
2,000
3,000
4,000
5,000
6,000
7,000
8,000
9,000
10,000
11,000
2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 min.
uV Max. Intensity: 10,525
Figure 1: Comparison of RF (black) with PDA detection (violet)
0123456789
101112131415
-10.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 min.
mV Max. Intensity: 10,525
Mobile phase A
Mobile phase B
Flow rate
Column oven temperature
Detection
Injection volume
1.0 % aqueous solutions of acetic acid
Acetonitrile
0.9 mL/min (40 Vol.-% B)
50 °C
PDA 280 nm, RF-20Axs Ex 280 nm, Em 325 nm
1 µL
Column Shim-Pack GIST C18 (2.1 x 100 mm i.D., 2 µm)
Table 1: Method parameters for analysis of capsaicin and dihydrocapsaicin
Table 2: Results of measurements of chili peppers
Home Grown
Habanero
Piri Piri
Bhut Jolokia
Sample
µg/g (sample)
1,501.4
1,693.4
4,877.7
24,356.1
µg/g (sample)
388.5
782.2
2,273.0
8,818.6
Capsaicin Dihydrocapsaicin
30,427
39,857
115,125
534,113
Scoville
11SHIMADZU NEWS 1/2018
APPLICATION
capsaicin is the peak eluting at2.84 min and the dihydrocapsaicinis the peak later eluting at 4.16 min.
Comparison of chili peppers and chili sauces
The two calibration curves of cap-saicin (figure 3 left) and dihydro-capsaicin (figure 3 right) serve as abasis for later determination of thecapsaicin content in the extractedchili peppers and the chili sauces.
For sample preparation of thedried chilies and sauces, a definedamount of sample is first weighed(1 g chili pepper, 2 g sauce) anddissolved in 10 mL ethanol. Afterone hour of extraction in a waterbath (100 °C) and filtration of thesolution, 1 µL is injected (figure 4).
In total, four chili peppers and fivesauces with distinct degrees ofpungency were examined. Figure5 shows the chromatogram of asauce with a pungency of levelseven, i.e. medium to high, inwhich capsaicin, dihydrocapsaicin
and also nordihydrocapsaicin canbe identified.
Formula for the degree of pungency
The calibration curves of capsaicinand dihydrocapsaicin are used forquantification. To determine thedegree of pungency, the concen-trations are ascertained accordingto the peak areas and converted tothe initial weight. The result canthen be converted to the Scovillescale using the formula below(without nordihydrocapsaicin) todetermine the degree of pungencyof chili peppers and sauces.
SHV = C + D +N
C = (µg capsaicin per gram) × 16,1D = (µg dihydrocapsaicin per
gram) × 16,1N = (µg nordihydrocapsaicin per
gram) × 9,3
The results are shown in tables 2and 3.
Summary
The method depicted shows aneasy sample preparation and fast
Table 3: Results of trial measurements of chili peppers and hot sauces
Figure 4: Sample preparation
0
100.000
200.000
300.000
400.000
500.000
600.000
700.000
800.000
900.000
1.000.000
1.100.000
1.200.000
1.300.000
0 10 20 30 40 50 60 70 80 90 100
Concentration Concentration
#2 CapsaicinArea
0
100.000
200.000
300.000
400.000
500.000
600.000
700.000
800.000
900.000
1.000.000
1.100.000
1.200.000
1.300.000
1.400.000
1.500.000
0 10 20 30 40 50 60 70 80 90 100
#3 DihydrocapsaicinArea
Figure 3: Calibration curves of capsaicin and dihydrocapsaicin
Filtration
Injection (1µL) in HPLC
Extraction in water bath(100 °C, 1 hour)
+ Ethanol 10 mL
Sample
analysis of chili products. Theresults obtained enable an approx-imate estimation of the expectedlevel of pungency, but due to thenon-inclusion of the nordihydro-capsaicin and a possibly incom-plete extraction, Scoville resultsare considered to be too low.
As expected, the results reveal asignificantly higher degree of pun-gency of pure chili peppers thanfor Currywurst sauces. This dif-ference is a result of the samesample processing for both types
of samples and the diluting effectof the sauce, which contains com-ponents of pure chili peppers.However, the goal was to makethe expected trend of pungencyvisible analytically for sauces withdifferent degrees of pungency, andthis has been achieved. This isclearly shown for the examples intable 3.
Literature[1] wikipedia.org/wiki/Currywurst
[2] wikipedia.org/wiki/Capsaicin
Sauce 3
Sauce 5
Sauce 7
Sauce 10
Sauce 10+
Sample
µg/g (sample)
5.9
6.8
405.6
1,103.2
4,867.0
µg/g (sample)
12.0
11.6
120.9
442.3
3,182.4
289
296
8,478
24,882
129,594
Capsaicin Dihydrocapsaicin Scoville
0
5
10
15
20
25
30
35
40
45
50
55
60
65
0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 min.
Max. Intensity: 77,955mV
Figure 5: Chromatogram of the sauce with pungency level 7
Further information
on this article:
• Application note:
Shimadzu Application
News No. L335
EM Wavelenght (nm) / EX Wavelenght (nm)
3000
10,000
20,000
30,000
40,000
400
500
600
700
250 300 350 400 450 500 550 600 650 700
APPLICATION
12 SHIMADZU NEWS 1/2018
Olive oil is top source of vitamin EA quantitative fluorescence analysis of tocopherols
and Greece to the United States,Australia and Japan [6, 7].
High sensitivity of fluorescencespectroscopy
Fluorescence spectroscopy is verysuitable for component analysis ofolive oils. The method has a high-er sensitivity than, for example,UV/Vis spectroscopy, since thesignal-to-noise ratio is significant-ly higher. Also, fluorescence spec-troscopy can be applied in threedimensions, which is an advantagefor particularly complex composi-tions of samples.
In 3D fluorescence spectroscopy,the associated emission spectra areapplied for a range of excitationwavelengths. Figure 2 shows a 3Dspectrum of commercial olive oil.In addition to the excitation wave-length, fluorescence activities in
the range of 290 - 340 nm, 350 -450 nm and 660 - 680 nm are present. The emission at around670 nm (Ex: 400 nm) is typical forchlorophyll, while the broad bandbetween 350 nm and 450 nm iscaused by polyunsaturated fattyacids and their oxidation products.The last remaining emission peakat about 320 nm is attributable tovitamin E [8].
The concentration of fluorescence-active chromophores in pure oliveoil is very high. In order to reducethe intensity of the fluorescence, itis possible to rotate the sample 30°or 60° to the excitation beam. Inthis way, the volume traversed bythe excitation beam is reduced.
However, this does not affectquenching effects within the sam-ple. In order to reduce this, oliveoil is diluted with n-hexane (1 vol.-% olive oil) for measure-ment. This also impacts on quan-tification of vitamin E in olive oil,since significantly fewer matrixeffects occur [4]. Figure 3 shows acomparison of the measurement ofa dilute hexane solution (1 vol.-%)with a higher concentration (30 vol.-%). The spectrum of thehigher concentrated oil-hexanesolution (black) clearly shows thematrix, in addition to the toco-pherol peak at about 320 nm,which makes it difficult to evalu-ate the peak area amongst others.
Quantitative assessment of vitamin E content
To quantify the vitamin E contentin olive oil, an external calibrationis performed. To test the dynamic
T ocopherols are methyl-sub-stituted chromanols with aside chain consisting of three
isoprenes. The four α-, β-, γ- andδ-tocopherols differ in the num-ber and position of the methylgroups in the phenolic part of thechroman ring. The α homologuecontains three methyl groups,while the β- and the γ-homo-logues are dimethylated positionalisomers. The δ homologue ismono methylated. These sub-stances all exhibit vitamin E activ-ity, but the biological potential ofR,R,R-α-tocopherol clearly sur-passes the other homologues with1.49 IU/mg [1].
Tocopherols are used, for exam-ple, in the food industry, becausethey effectively inhibit fat oxida-tion in food [2]. This effect is alsoevident in other biological systemssuch as the human body.
20 % of vitamin E requirements are contributedby fats and oils
The largest sources of vitamin Eare vegetable oils. Based on datafrom the National Health andNutrition Survey (NHAVES II), it is evident that fats and oils con-tribute more than 20% to vitaminE requirements [1]. The daily dose
required increases when the dietcontains a large proportion ofunsaturated fatty acids. For exam-ple, the necessary α-tocopherolconsumption is 0.09 mg/g formonounsaturated fatty acids and0.4 - 0.6 mg/g for diunsaturatedfatty acids [3]. According to the
National Research Council (1989),a 10 mg daily intake of vitamin Efor men and 8 mg for women isrecommended.
According to nutritional beliefs,extra virgin olive oil, despite itshigh content of monounsaturatedfatty acids, is suitable for supple-menting the daily vitamin E intakeand for protection from vitamin Edeficiency [4, 5]. Today, it is rec-ognized worldwide as a healthpromoting oil, which is why extravirgin olive oil is becoming increas -ingly important in many coun-tries. As a result, large volumes ofoil are exported from Italy, Spain
Figure 1: Chemical structure of α-tocopherol
Figure 2: 3D scan of hexane diluted olive oil (1 vol.-%)
Figure 3: Range of diluted olive oil 1 % v/v, in n-hexane (purple), spectrum of diluted
olive oil 30 % v/v, in n-hexane (black)
Intensity
nm250.0 300.0 400.0 500.0 550.0
0
-290.9
1,000.0
2,000.0
3,000.03,350.2
APPLICATION
SHIMADZU NEWS 1/2018 13
range, calibration solutions with0.6 - 75 ppm α-tocopherol pre-pared in hexane are used andmeasured at an excitation wave-length of 290 nm. It is noticeablethat the sensitivity to the higherα-tocopherol concentrationsdecreases, so a calibration in therange of 1 - 20 ppm is therefore themost suitable.
All measurements were also donewith the synchronous technique.Excitation and emission wave-lengths were scanned, with bothwavelengths at a constant distancefrom each other. Excitation peakin the spectrum was significantlyattenuated, as well as second order light and matrix effects ofthe sample. This resulted in muchnarrower peaks. These are usuallyeasier to evaluate, but have a low -er intensity [9].
Normal and synchronous measurement
For testing, an olive oil-hexanesolution (1 vol.-%) was measurednormally and synchronously. The α-tocopherol peak is verysmall, so that the sample can bearranged at the lower end of thecalibration line. Oil-hexane solu-tion thus contains approximately1 - 2 ppm α-tocopherol, while aslightly higher value is deducedusing calibration with synchro-nous technology. For a reliablecalibration, it is recommended toincrease the proportion of oliveoil in the hexane solution by a fewpercent. A compromise between
good quantifiability and as fewmatrix effects as possible for theolive oil concentration has to befound.
Additionally, fluorescence spectraof hexane solutions with higher α-tocopherol concentrations havebeen measured in order to seehow the fluorescence reacts athigher concentrations. The result-ing plot of intensities versus con-centration (figure 6) shows thatabove a concentration of 100 ppm,quenching effects occur within thesample and a linear correlationbetween intensity and concentra-tion is no longer present. There -fore, it makes no sense to measureundiluted olive oil.
Summary
Vitamin E is a quality feature ofolive oil, but quantification byfluorescence spectroscopy is chal-lenging. In general, sufficient dilu-
Intensity
Concentration of �-tocoperol in ppm0.00 5.00 10.00 15.00 20.00 25.000
500
1,000
1,500
2,000
2,500
3,000
3,500
4,000
Figure 4: Calibration of α-tocopherol in hexane normal and with the synchronous
technique and respective calibration lines
Synchronus
––– Linear (synchronus)
––– Linear (normal)
Normal
Intensity
nm
260.9 300.0 400.0 500.0 600.0 710.0
0-207.3
1,000.0
2,000.0
3,000.0
Figure 5: Fluorescence spectrum of an olive oil sample (black); Synchronous scan of
an olive oil sample (red)
tion of the olive oil with hexane tominimize quenching within thesample and to ensure system cali-bratability is necessary. However,the sample should only be dilutedto the extent that the α-tocophe -rol concentration is still approxi-mately 10 - 15 ppm. For sampleswith a high amount of matrix, itmay be useful to measure the flu-orescence in synchronous mode,as it minimizes interfering effects.
AuthorsAurelia Bertini, Hochschule Niederrhein
Manos Barbounis, Asteriadis S.A.
Vassilis N. Kamvissis, Sevitel
Literature[1] Eitenmiller, R. R.; Landen, WO, Jr.
Vitamin E. Tocopherols and tocotrienols.
In Vitamin Analysis for the Health and
Food Sciences; CRC Press: Boca Raton,
FL, 1999; p 109.
Intensity in a.U.
Concentration of tocoperol in ppm50 70 90 110 130 150 170 190 210
4,000
5,000
6,000
7,000
8,000
9,000
10,000
11,000
Figure 6: Calibration of an α-tocopherol-hexane solution in the range of 80 - 200 ppm
(Ex: 290 nm)
Synchronus scan
Normal
[2] Kamal-Eldin, A; Andersson, R.
A multivariate study of the correlation
between tocopherol content and fatty
acid composition in vegetable oils.
J. Am. Oil Chem. Soc. 1997, 74,
pp. 375-380.
[3] Belitz, HD; Grosch, W.
Food Chemistry, 2nd Ed.; Spinger publish-
ing house: Berlin, Germany, 1999.
[4] Kafatos, A; Comas, G.
Biological effects of olive oil on human
health. In Olive Oil; Kiritsakis, AK, Ed.;
American Oil Chemists’ Society: Cham -
paign, Il, 1990; Chapter 17, pp. 157-181.
[5] Lenart, EB; Willet, WC; Kiritsakis, AK.
Nutritional and Health aspects of olive
oil. In Olive Oil Kiritsakis AK Ed:
Food and Nutrition Press: Trumbull CT,
1998; Chapter 16, pp. 299-322.
[6] Petrakis, C.
Good Manufacturing Practice (GMP)
guidelines for virgin olive oil production.
Grasas Aceities 1994, 45, pp. 53-54.
[7] Eleni Psomiadou, Maria Tsimidou,
Dimitrios Boskou, a-tocopherol Content
of Greek Virgin Olive oils, J. Agric. Food
Chem., 2000, 48 (5), pp. 1770-1775.
[8] Kyriakidis & Skarkalis:
Journal of AOAC Internattional Vol. 83,
No. 6, 2000.
[9] Sikorska E., Khmelinskii I., Sikorski M.,
Analysis of Olive Oils by Fluores cence
Spectroscopy: Methods and Appli cations,
InTech (2012).
0.00
0.01
0.02
0.03
0.04
0.05
0.06
0.0 2.5 5.0 7.5Concentration ratio
Acetaldehyde
Area ratio (x 100)
0.0
1.0
2.0
3.0
4.0
5.0
6.0
0.0 2.5 5.0 7.5Concentration ratio
Isobutanol
Area ratio
0.00.10.20.30.40.50.60.70.80.9
0.00 0.05 0.10 0.15Area ratio
Diacetyl
Con
centration
ratio
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.0 0.1 0.2 0.3 0.4 0.5Area ratio
2,3-pentanedione
Con
centration
ratio
APPLICATION
14 SHIMADZU NEWS 1/2018
levels, they give off an unpleasanttaste and smell.
This shows that rapid and reliablemethods are highly desirable for determination of aroma pro-file of the beer due to its impor-tance.
B eer flavor is formed by acomplex mixture of manycomponents giving each
brew its own distinctive personali-ty. This mixture mostly includesalcohols, esters, acids, sulphurcompounds and vicinal diketones.
Esters represent one of the mostimportant flavor groups and playa considerable role in the organo -leptic characteristics of the beer.Production of esters is influencedmainly by wort composition andfermentation parameters duringthe brewing process. Additionally,esters are often the target-com-pounds in authentication andquali ty control methods.
Furthermore, monitoring for vici-nal diketones (VDKs) including
Dimethyl sulphide (DMS) is a sul-fur compound with the taste andaroma of sweet corn. This deriveseither from the malt (as a result offermentation pro cess) or bacterialinfection. Sulfur componentscould be considered acceptable atlow concentrations, but in higher
2,3-butanedione (diacetyl) and2,3-pentanedione, is also a criticalstep in determination of flavor inbeer. VDKs are considered to beextremely important since theyare known to affect the taste ofthe beer. These components areresponsible for the sweet butterflavor and are considered as non-beneficial at high levels.
Another important task (in thebrewing process) is monitoring ofacetaldehyde. As known, acetalde-hyde is reduced to ethanol by yeastduring secondary fermentation,but this process may be reverseddue to extensive oxidation, con-verting ethanol back to acetalde-hyde. Acetaldehyde can also be aproduct of bacterial spoilage causedby Zymomonas or Acetobacter.
Flavors in beer determined by Headspace-GCGC-2010 Plus in the Quality Controlprocedure of a large Greek brewery
Figure 1: Typical calibration curves Figure 2: Analysis of VDKs in a standard
-0.5
0.0
0.5
1.0
1.5
2.0
2.5
2.0 3.0 4.0 5.0 6.0 7.0
uV (x 10,000)
Minutes
mixture&ISTD9.gcd
mixture&ISTD8.gcd
mixture&ISTD7.gcd
mixture&ISTD6.gcd
mixture&ISTD5.gcd
mixture&ISTD4.gcd
mixture&ISTD3.gcd
mixture&ISTD2.gcd
mixture&ISTD1.gcd
Average
%RSD
Maximum
Minimum
Standard deviation
4.249
4.249
4.248
4.248
4.247
4.247
4.246
4.245
4.243
4.247
0.049
4.249
4.243
0.002
36,193
36,457
36,336
36,657
36,830
36,652
36,530
36,923
35,667
36,472
1.038
36,923
35,667
379
5.552
5.551
5.551
5.550
5.549
5.548
5.547
5.546
5.543
5.548
0.052
5.552
5.543
0.003
89,233
89,539
89,407
91,125
91,484
90,068
89,663
90,701
88,497
89,971
1.075
91,484
89,497
967
mixture&ISTD9.gcd
mixture&ISTD8.gcd
mixture&ISTD7.gcd
mixture&ISTD6.gcd
mixture&ISTD5.gcd
mixture&ISTD4.gcd
mixture&ISTD3.gcd
mixture&ISTD2.gcd
mixture&ISTD1.gcd
Average
%RSD
Maximum
Minimum
Standard deviation
ID#1 Compound name: Diacetyl
Titel Ret. time Area
ID#2 Compound name: 2,3-pentanedione
Titel Ret. time Area
Diacetyl
2,3-pentanedione
Acetaldehyde
Dms
Acetone
Ethyl formate
Ethyl acetate
Methanol
Ethyl propionate
Propanol
Isobutanol
Isoamyl acetate
Amyl alcohols
Ethyl capronate
0.9995
0.9999
0.9984
0.9989
0.9989
0.9976
0.9987
0.9965
0.9984
0.9991
0.9989
0.9965
0.9986
0.9973
1.04
1.08
2.51
2.20
1.3
2.25
1.30
2.43
1.75
2.89
2.50
1.35
2.85
2.93
Compound Correlation Coefficient RSD (%)
Injector temperature: 135 °C
Split ratio: 3
Column oven: 75 °C for 12 min
FID temperature: 150 °C
Pressure: 35 KPa
Carrier gas: Helium
Injector temperature: 135 °C
Split ratio: 3
Column oven: 35 °C (25 min), 10 °C/min
to 150 and hold 10 min
FID temperature: 150 °C
Pressure: 73 KPa
Carrier gas: Helium
Line 1 (VDKs) Line 2 (Esters)
15SHIMADZU NEWS 1/2018
APPLICATION
Worldwide established:Headspace-GC
Headspace sampling coupled withgas chromatography (HS-GC) is a widely used technique for theanalysis of beer throughout theworld. It is also considered im -portant in quality control (QC) in order to identify problems orchanges occurring in brewing orfermentation processes that couldaffect the quality of the finalproduct, i.e.:
• significant increases of ethyl for-mate, acetone and/or methanolin cases of contamination causedby inadequately disinfected tanksor leaks in cooling systems
• an abnormal increase in ethylcapronate related to yeast andfermentation problems.
The aim of this current work wasthe successful development of theHS-GC technique to successfullyimplement it in the Quality Con -trol of a large brewery in Greece.
Sample preparation
Beer samples require degassingprior to headspace analysis fortwo reasons. Firstly, it is criticalto prevent dissolved carbon diox-ide (CO2) from influencing vialpressure during the headspaceheating process, and secondly,CO2 eluting during chromatogra-phy disturbs the GC baseline.
Samples were prepared by trans-ferring the beer to a wide mouthbeaker and sonicating them brief -ly. After degassing, 2.5 mL of beersample was placed into a 20 mLheadspace vial, the internal stan-dard was added with a gas tightsyringe, and the vial was sealedwith a rubber septa. It was thenplaced in the rack of the head-space autosampler for incubationand injection.
Instrumentation
Gas chromatographShimadzu GC-2010 Plus, twoSplit/Splitless injectors, two lines,one with an ECD detector (analy-sis of VDKs) and the second with
a FID detector (analysis of esters,DMS, acetaldehyde).
Headspace autosamplerShimadzu AOC-5000 with a 2.5 mL headspace syringe.
Capillary columns • Line 1 (VDKs): Varian CP SIL
8 CB column (50 m, 0.53 mmID and 1 µm film thickness)
• Line 2 (esters): Varian CP Wax52 CB column (60 m, 0.32 mmand 1.20 µm film thickness)
Results and discussion
Following the identification of thecompounds, calibration was car-ried out using an aquatic solutionof 5% in ethanol. The substancesused for each analysis were as fol-lows:
• VDKs: diacetyl and 2,3 pentane-dione and 1,2-dichloropropaneas internal standard.
• Esters etc: acetaldehyde, DMS,acetone, ethyl formate, ethylacetate, methanol, ethyl propi-onate, propanol, isobutanol,isoamyl acetate, amyl alcoholsand ethyl capronate and n-buta -nol as internal standard.
The calibration curve used foreach substance consisted of sevenpoints, and the correlation coeffi-cients (r2) are listed in table 2,varying from 0.9965 to 0.9999.Some typical calibration curvesare also shown in figure 1.
Experimental data
Nine repetitions of the highestconcentration VDKs standardwere performed, and the relativeRSDs are shown in table 3.Repeatability was very good andin all cases RSD was less than 3%(see also table 3).
Conclusion
The headspace-GC technique is afast and reliable method for rou-tine analysis of odor compoundsin beer. Due to minimum samplepretreatment, high sensitivity and excellent repeatability of the Shimadzu GC-2010 Plus gaschromatograph and Shimadzu �
Table 1: Method parameters
Table 2: Correlation coefficients of the related substances
Table 3: Repeatability data of VDKs (screenshot from GC Solution software)
READ FOR YOU
APPLICATION
16 SHIMADZU NEWS 1/2018
AOC-5000 autosampler, it wasquite easy to implement it in theQuality Control procedure of alarge brewery plant in Greece.
This application can be done in the same way using the new Nexis GC-2030.
AuthorsManos Barbounis, Dimitris Georgantas
Application Laboratory, N.Asteriadis S.A.,
31 Dervenion Str. & Poseidonos Str., 144 51
Metamorfossi – Athens, Greece
E-mail: [email protected]
Literature[1] Tomáš Horák, Jirí Culík, Vladimír Kellner,
Marie Jurková, Pavel Cejka, Danuša
Hašková and Josef Dvorák, J.
-0.5
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.0 10.0 15.0 20.0 25.0 30.0 35.0 40.0
uV (x 10,000)
Minutes
Inst. Brew. 116(1), Analysis of Selected
Esters in Beer: Comparison of Solid-Phase
Microextraction and Stir Bar Sorptive
Extraction, pp. 81-85, 2010.
[2] Li Huimin, Li Hongjun, Liu Xiuhua,
Chen Bing
Int J Agric & Biol Eng, 21 (Vol. 5),
Analysis of volatile flavor compounds in
top fermented wheat beer by headspace
sampling-gas chromatography, 2012.
Figure 3: Analysis of esters etc. in a standard
Guardian in the chemical parkTOC process measurement at Leuna Chemical Park, Germany
which is passed through the sam-ple.
This sample preparation is doneautomatically by the TOC-4200.Once the inorganic carbon isremoved, an aliquot is injectedautomatically onto a 680 °C plat-inum catalyst where all existingorganic compounds are oxidizedto carbon dioxide. The resultingCO2 is conducted by a carrier gasflow to a highly sensitive CO2-selective NDIR detector and sub-sequently measured. Based on anexternal calibration, the TOCconcentration is then calculated.
Wastewater treatment
At the chemical site of Leuna,about 300 m3 per hour of waste-water is produced that needs to be cleaned. For this purpose, thesite operates its own multi-stagewaste water treatment plant. Inorder to protect the biologicaltreatment stage of the sewagetreatment plant, the entrance of
A s a method of analysis thathas been established fordecades, the sum parameter
TOC (Total Organic Carbon)measures the total contaminationof organic components in a matrixin a single analytical run – wheth -er in a laboratory environment oronline during an industrial pro -cess. This makes the TOC a ver -satile and universal parameter, asdemonstrated by InfraLeunaChem ical Park in Leuna, Germany.
The Leuna Chemical Park, locatedin the heart of central Germany,stands for dynamism, innovationand maximum efficiency. As anindependent operator of the entireinfrastructure, InfraLeuna ensuresthe synergy of the Leuna chemicalsite and provides the frameworkfor local companies for a cost-effective and efficient production.
The comprehensive offer ofInfraLeuna consists of the redun-dant provision of steam, electrici-ty, fresh water and drinking water
An automatic sampling stationwithdraws process water steadilyand feeds it to the analyzer. It isimportant to adjust the extractionto the respective water quality: If it contains particles, it has to betreated differently than saline par-ticle-free water. Shimadzu offersvarious sampling modules for thispurpose. Up to six different sam-ple streams can be connected toone station and can be measuredby a single analyzer.
Important for the determinationof the TOC is the differentiationbetween organic and inorganiccarbon. After all, carbonates andbicarbonates can be found inevery natural water. The mostcommonly used method for TOCdetermination is therefore the so-called NPOC (Non Purge ableOrganic Carbon) method. Thesample is acidified in order toconvert the carbonates and bicar-bonates contained to CO2. Sub -sequently, the resulting carbondioxide is expelled by a gas stream
as well as sanitation and otherservices. This also includes com-plex logistics services. The focus is on the business success for thecustomers and the further devel-opment of the chemical site as awhole.
Analytical monitoring of waterquality is an integral part of theseservices. It is an important toolfor safe running of all processes,and protection of equipment andthe environment. It is carried outat various points where differentwater qualities occur, such aswaste water, ultrapure water orwater vapor.
The TOC
To quickly measure the level oforganic component contaminationin water, the TOC value is deter-mined. This can be done offline inthe lab as well as online during theprocess. Shimadzu’s TOC-4200 isan example of a TOC process foronline monitoring.
READ FOR YOU
17SHIMADZU NEWS 1/2018
Further information
on this article:
• www.laborpraxis.
vogel.de/per-toc-
messung-im-prozess-
die-wasserqualitaet-im-chemiepark-
ueberwachen-a-669678/
the biological treatment stage ismeticulously controlled. An on -line TOC system closely monitorsthe inflow, as excessive amountsof organic load can severely dis-rupt or even kill the plant’s sensi-tive biology. In order to detectpotential incoming volatile solventloads, NPOC and also POC(purgeable organic carbons) asoption are measured in the feed.
To control the efficiency of thewastewater treatment plant andthe clarification process, output of the wastewater treatment plantis also monitored. For this, twostreams are analyzed:• waters from the various purifi-
cation stages of the sewage treat-ment plant
• surface waters resulting fromprecipitation events.
If the appropriate limits are notexceeded, the water may be dis-charged to the river. To avoidenvironmental damage, the TOC-4200 systems used for thispurpose are connected to a me -chanical gate valve system. If thelimit value is exceeded, the valve isclosed automatically and the wateris sent to a containment tank andthen returned to wastewater treat-ment.
Ultrapure water
In many areas of the chemicalpark, ultrapure water is used,either for chemical processes orfor thermal processes in wasteheat or boiler plants. InfraLeunaproduces about 350 m3 ultrapurewater per hour. In this manufac-turing process, different tech-niques are combined. The raw
water is first decarbonated, fil-tered through a gravel filter and a candle filter, then purified byreverse osmosis and desalted byion exchange.
TOC impurities in ultrapurewater can have a negative impacton chemical processes. Especiallyin the production and processingof high purity chemicals, contami-nation can have a negative influ-ence on the quality of the product.An important specification ofultrapure water is thereby de -scribed by the TOC: it must notcontain more than 0.2 mg/L oforganic carbon. The ultrapurewater is therefore examined con-tinuously before feeding into thesupply lines. To perform such sen-sitive measurements, a specialhigh-sensitivity catalyst is used.
The platinum-plated quartz woolof the catalyst enables injection ofhigher volumes. Detection limitsbelow 50 µg/L TOC are achievedin this combination.
Steam / condensate
One of the most important sourc -es of energy in the Leuna Chemi -cal Park is steam. It is used to heatreactors and is sometimes evenpart of the manufacturing process.InfraLeuna supplies their custom -ers and their own plants withsteam at different pressure levels.The steam is generated with highefficiency, using cogeneration sys-tem in a combined cycle powerplant.
Contaminants in the water usedfor steam production can havenegative effects on the plant. In
addition to inorganic substancessuch as salts or CO2, organic con-taminants can also cause damage.In steam generation, some organicsubstances are decomposed. De -composition products, e.g. organicacids, lead to increased corrosionof system components such asheat exchangers or the blades ofsteam turbines.
In the return condensate, organicsubstances can accumulate. Thecondensate is therefore also moni-tored and only reused if a maxi-mum limit of 0.8 mg/L TOC ismet. If the measured TOC con-centration is higher, the conden-sate is treated by suitable proce-dures before reuse. To protect thesystem components in the steam-condensate circuit, TOC is care-fully monitored.
Recooling Water
For condensation in the water-steam circuit, additional coolingcircuits are needed. The coolingtowers used for this purpose withtheir large amounts of water arean open system, in contrast to theclosed water-steam circuits. Fromthe outside, various environmentalinfluences affect the water qualityof the so-called recooling water.In addition, with temperaturesbetween 20 °C and 40 °C, it pres-ents an ideal breeding ground formicroorganisms of all kinds. Toreduce microbial contamination,chemicals are added to the recool-ing water. This water is also moni-tored continuously for its organicimpurity level.
Sampling
At the Leuna chemical site, pro -cess TOC devices are used inmany places to monitor the water.Sampling, on the other hand, iscarried out in all used systems bymeans of counter flow-extraction.The sampling system consists of a curved overflow pipe into whicha sampling capillary is inserted.
The sampling point is locateddirectly behind the pipe bend, sothat a turbulent flow of the sam-ple homogenizes a multiphasemixture which may be present.The TOC-4200 draws the flowingsample out of this capillary againstits direction of flow, and then
washes it back with rinse water.The sampling device thus containsno moving parts or filters and iseffectively maintenance free. Theflowing medium flushes particlesor deposits away from the capil-lary, so that no blockages canoccur.
Conclusion
Many varied fields of applicationwith TOC analysis are in opera-tion in a chemical park such as in Leuna. Whether sewage, rain-water, condensate, ultrapure wateror recooling water, whether withor without salts and particles – allwaters have their own require-ments for analysis, which can bemet by appropriate options.
Read for you in LaborpraxisDecember 2017
Analytical monitoring of water quality by TOC measurement is essential for efficient
processes in the Leuna Chemical
IMPRINT
Shimadzu NEWS, Customer Magazine of Shimadzu Europa GmbH, Duisburg
PublisherShimadzu Europa GmbHAlbert-Hahn-Str. 6 -10 · D-47269 DuisburgPhone: +49 - 203 - 76 87-0 Fax: +49 - 203 - 76 66 [email protected]
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Circulation German: 6,400 · English: 4,120
CopyrightShimadzu Europa GmbH, Duisburg, Germany – March 2018.
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LATEST NEWS
18 SHIMADZU NEWS 1/2018
Video tutorials using the new GC generation Nexis GC-2030 as an example
Troubleshooting via YouTube
R egular analysis of customerrequests from around theworld revealed that users
would like easier access to GCanalysis and simplification ofdaily maintenance tasks, such aschanging the column.
With its new troubleshootingchannel on YouTube, Shimadzutakes a new approach using videoand voice to give practical tips &tricks relating to chromatography.The Nexis GC-2030 as part of the new GC generation is used asan example to show how thishigh-precision technology can beconveniently maintained and justhow easy daily work with theNexis GC-2030 really is.
Consistent user guidance
Self-explanatory icons on the GC-2030 color touchscreens guideusers intuitively through the pro-cedure for setting up all requiredmethod parameters. The sameicons and structure of the typicalGC modules are also used in theLabSolutions software. The“LabSolutions Direct” interfacecan be used to see the status of arunning GC analysis as well asremotely restarting sample meas-urements using a tablet PC orsmartphone, provided the
GC-2030 has network access (figure 1).
Simple maintenance
Another video shows just howeasy it is to change the septumand liner as part of routine main-tenance work on the GC injector(figure 2). After the work is com-plete, the simple diagnostic func-tion of the GC-2030 providesclear information on whether theinjector is again gas-tight andready for use.
Changing the column is a standardprocedure if the GC is used fordifferent types of applications(figure 3). The unique Click-Tektechnology reduces this procedureto a few well-defined steps. Asimple snap hook mechanism issufficient to verify whether the
column has been installed correct-ly as there are only two possiblepositions: “open” and “shut”.Furthermore, an optional LEDoven lamp gives a clear viewinside the GC-2030 oven.
Replacing the gas filter in the lineof the split gas outlet is carriedout less frequently, but can also be done quickly without a tool(figure 4). The filter prevents con-tamination of the electronic unitcontrolling the carrier gas. Anindicator in the filter changescolor when replacement is neces-sary.
These videos can be watched sim-ply by clicking on the links in theShimadzu News App.
Alternatively, “GC-2030” can beentered in the search mask ofYouTube.com.
An additional video tutorial de -tails changing of the desolvationline on the LCMS-8060 triple-quad mass spectrometer. Morevideos will be added soon.
Figure 1: YouTube: Touchscreen display & LabSolutions Direct
Figure 4: YouTube: Filter Nexis GC-2030
Figure 3: YouTube: ClickTek and oven lamp
Figure 2: YouTube: Septum and Liner
Further information
on this article:
• bit.ly/
Troubleshooting_
ShimadzuEurope
READ FOR YOU
19SHIMADZU NEWS 1/2018
A n international collaborativeresearch team led by theJapanese National Center
for Geriatrics and Gerontology(NCGG), Koichi Tanaka MassSpectrometry Research Laboratoryat Shimadzu Corporation, and theAustralian Imaging, Biomarkerand Lifestyle Study of Aging(AIBL) groups has established ahighly sensitive blood test able to identify individuals at risk ofdeveloping Alzheimer’s disease.(The research also involved collab-orators at The University ofTokyo, Kyoto University, KindaiUniversity, and Tokyo Metropo -litan Institute of Gerontology.)The results have been publishedonline, on 31 January 2018, inNature, one of the world’s leadingscientific journals.
One of the essential pathologicalsignatures of Alzheimer’s disease isdeposition in the brain of an ab -normal protein, called A�-amyloid(A�). About three decades beforethe onset of dementia symptoms,the deposition starts silently, with-out any sign of cognitive abnor-malities. It is estimated that about20 - 40 % of the general elderly
population have a significant A�
burden in their brain. While theAβ deposition does not necessarilymean a fast progression to Alzhei -mer’s dementia, these individualsare considered to be “at risk” ofdeveloping Alzheimer’s disease atsome future point. The new bloodtest can identify individuals withabnormal A� deposition in thebrain,with about 90 % accuracy.
“Currently, only positron emissiontomography (PET) imaging orcerebrospinal fluid testing areavailable to ascertain brain A�
burden, however, these tests areexpensive and/or invasive” saysAkinori Nakamura, LaboratoryChief at NCGG. “Therefore, aminimally invasive and cost-effec-tive blood test is strongly desired;however, it has proven to be verydifficult to develop despite muchresearch effort. Our study is im -portant because it not only demon -strates the high performance ofthis blood test, but also its reliabil-ity and reproducibility as it wassuccessfully validated in two inde-pendent large datasets from differ-ent countries, Japan (121 samples)and Australia (252 samples).”
One key point for their success isthat the test employed a new meth -od called immunoprecipitation andmass spectrometry (IP-MS). “Fromonly 0.5 mL of a blood sample, theIP-MS method can quantitativelymeasure several A�-related pep-tides, such as A�1-42, A�1-40, andAPP669-711, in plasma, eventhough their concentration in plas-ma is extremely low. We foundthat the ratio of these peptides,APP669-711/A�1-42, A�1-40/
A�1-42, were anaccurate surrogatefor the brain A�
burden. This tech-nique was estab -lished by our col-league NaokiKaneko, who alsofirst found APP669-711 in plasma,” saysKoichi Tanaka atShimadzu Corpo ra -tion, who achievedthe Nobel Prize inChem istry in 2002for developing amethod for massspectrometric anal -yses.
Less than a teaspoon of blood can predict Alzheimer’sdisease risk
“Scientists at Shimadzu Corpora -tion will need to scale up the testso that it can be widely used, butonce this issue is resolved, this newtest has the potential to eventuallydisrupt the current PET/CSF tech-nologies. In the first instance, how -ever, it is likely to be used forscreening,” says Colin L. Masters,Professor at the Florey Institute,The University of Melbourne, wholed the AIBL project.
“Our blood test may also have atransformative potential to facili-tate the development of effectivedrugs for Alzheimer’s disease,”says Katsuhiko Yanagisawa,Director-general of ResearchInstitute at NCGG. He continues,“Although drugs for Alzheimer’sdisease are still under develop-ment, the best chance for the effi-cacious interventions are consid-ered to be before the onset of thedementia symptoms. Our bloodtest is expected to enable popula-tion-based screening to identify“at risk” individuals to be recruit-ed in preclinical and prodromalprevention trials with reasonablecost-benefit and scalability.”
Authors of the article, publishedin Nature:
Akinori Nakamura, Naoki Kaneko, Victor L.
Villemagne, Takashi Kato, James Doecke,
Vincent Doré, Chris Fowler, Qiao-Xin Li, Ralph
Martins, Christopher Rowe, Taisuke Tomita,
Katsumi Matsuzaki, Kenji Ishii, Kazunari Ishii,
Yutaka Arahata, Shinichi Iwamoto, Kengo Ito,
Koichi Tanaka, Colin L. Masters & Katsuhiko
Yanagisawa
Koichi Tanaka at Shimadzu Corporation,
who achieved the Nobel Prize in Chemistry
in 2002 for developing a method for mass
spectrometric analyses
Further information
on this article:
• www.nature.com/
articles/nature25456
20
analytica
Munich, GermanyApril 10 - 13, 2018www.analytica.de
Wire
Düsseldorf, GermanyApril 16 - 20, 2018www.wire.de
ISCC
Riva del Garda, ItalyMay 13 - 18, 2018www.iscc42.chromale-ont.it
IFAT
Munich, GermanyMay 14 - 18, 2018www.ifat.de
EPRW
Munich, GermanyMay 22 - 25, 2018www.eprw2018.com
Automotive TestingExpoStuttgart, GermanyJune 05. - 07, 2018www.testing-expo.com
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LATEST NEWS
Pop the corks: 50th anniversaryof Shimadzu in EuropeTime to celebrate
Quiz ‘n’ Win
Throughout the year, Shimadzutakes the opportunity to cele-brate with its clients and thebusiness communities. In thecoming months, exciting com-petitions will be run with lotsof attractive prizes to win. Justvisit the www.shimadzu.eu/50th-anniversary websiteand apply to take part in thequiz with questions aroundShimadzu’s history, portfolioand milestones. Don´t worry,you don´t have to be an expert!Good luck!
T his year, Shimadzu celebratesthe 50th anniversary of itspresence in Europe. This is
an exciting year with lots of inno-vations to be expect ed, and it isalso a time to celebrate with theclients, employees and the busi-ness communities of analyticalinstrumentation and medical tech-nology.
It started in 1968 with five employ -ees: Shimadzu Europa commencedoperations in Düssel dorf, the capi-tal of Ger many’s most populousfederal state. In 1987, after 20years of growth, Shimadzu relo-cated a few miles further to Duis -burg, a city with the largest inlandport in Euro pe, which since thenhosts Shimadzu’s Euro pean Head -quar ters for the Shimadzu Corpo -ration (Kyoto, Japan). Today,Shimadzu em ploys almost 700people in Europe and has devel-oped into a large European net-work with offices and trade part-ners in 81 cities from 48 countries.
“Excellence in Science”
The headquarter in Duisburg pro-vides the technological and appli-
cation-oriented knowhow.Through trainings and seminars inthe over 1,500 sqm Laborato ryWorld, it is regularly shared withthe sales and service forces whotransfer it into the markets. Theyare one of the world’s largest pro -viders of analytical instrumenta-tion and X-ray diagnostic imagingsolutions. Whereas medical tech-nology covers Angiography, Fluo -roscopy and Radiography as wellas Mobile X-ray Systems, the ana-lytical instrumentation focuses onadvanced solutions in Chromato -gra phy, Mass Spec trometry, Spec -troscopy, Total Organic Carbonanalysis, Imag ing, Life Sciences,Material Test ing and MeasuringTechnology.
“Excellence in Science” stands forShimadzu’s core value propositionrepresenting the company’s scien-tific and technological approach toalways providing business, medical and research solutions with ad -vanced analytical and diagnosticimaging systems, ensuring betterconsumer, patient and environ-ment protection as well as productsafety. Numerous world firstswhich have meanwhile become
industrial and clinical standardstoday substantiate this tag line.
Paradigm shifts in business
Developing, running and growinga company for 50 years (and on aglobal scale it is more than 140years) is not just a question ofoffering the right products and
services, it is also a matter ofadapting successfully to societal,political, econom ic and technolog-ical changes as well as aligning toclients’ expansion plans, needs andstructures to fully support theircompetitiveness. These all influ-ence the ways of doing business,cooperating with clients and driv-ing a company.
Just to mention a few: the digitalrevolution, i.e. the transition fromthe industrial era to the informa-tion age, caused a technologicalparadigm shift regard ing newapplications, precision and con-ducting systems. A similar impactin a political context was the raiseof the Iron Cur tain which gaveaccess to new markets and targetgroups, and also led to a newpolitical and market order all overEurope.