shimadzu lunch seminar · shimadzu lunch seminar "from water to wine" - analytical tools...
TRANSCRIPT
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Shimadzu Lunch Seminar
"From Water to Wine" - analytical tools for determination of
contaminants in food and environmental samples using atomic
spectroscopy
Pau, 04.02.2019
Uwe OppermannShimadzu Europa GmbH, Duisburg
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ICPMS the high sensitivity add-on to your analytical toolbox:
Determination of contaminants in food and food packaging
Uwe OppermannShimadzu Europa GmbH, Duisburg
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Food Market Place Europe
⚫ Market Size 1109 bn € ( )
⚫ Biggest industry segment in EU (15.2%)
⚫ 294000 Companies
⚫ R & D Invest 2.9 bn € ( )
Data & Trends of the European Food Industry Oct. 2018, Copyright: FoodDrink Europe, Brussels
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„Top 10“ in Europe/ World
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Alcoholic Beverages in Europe (TO)
https://de.statista.com/outlook/10000000/102/alkoholische-getraenke/europa#market-revenue
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The „Alcohol Belts“ in Europe
https://en.wikipedia.org/wiki/Alcohol_belts_of_Europe
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Quality Control
Is our food safe ????
⚫ Nobody can answer this question …….
⚫ ….. but It has never been ckecked better than today
⚫ EFSA: More than 97% of food in the EU contains Pesticide residues with the tolerance limits: https://www.efsa.europa.eu/en/press/news/150312
⚫ 97.4% below the max. allowable concentration
⚫ 1.5% above the allowable concentration
⚫ EFSA (2016): 27 of 28 EU-Memberstates reported 710.000 samples
⚫ The failure rate for Metal Contaminants was higher than in other classes (> 5%)
https://efsa.onlinelibrary.wiley.com/doi/epdf/10.2903/sp.efsa.2018.EN-1358
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Results after Determination
Published results of LGL in Bavaria:
⚫ Fruit spirits
⚫ Number of samples: 159
⚫ Claims: 77 (48,4 %)
⚫ Reason of claim:
⚫ Wrong declaration
⚫ High concentration of Ethyl acetate, Propanol-1, Butanol-2
⚫ Particles from Filter material Asbestos, Glas und Chrysotil fibres
⚫ Metal contaminants such as copper
https://www.lgl.bayern.de/lebensmittel/warengruppen/wc_37_spirituosen/index.htm
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Properties to determine:
• Composition
• Essential Elements
• Toxic Elements
• Taste, Color.....
• Contaminants
Food Quality…….
Laws and Regulations:
• Drinking Water Regulation
• Beer Purity Law
• Foodstuff and commodity Act
• European Food Law
• European Food Safety Authority
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More Regulations…..
⚫ Regulation (EU) 1881/2006 setting maximum levels for certain contaminants in foodstuffs
⚫ European Wine Regulation from 9. May 2012
⚫ Mineral- and Tablewater- Regulation 1. August 1984 (BGBl. I S. 1036) witharticle 25 from 5. July 2017
⚫ etc…..
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One Stop Vendor in Food Analysis
A
Z
AAS
ICP-OES/MS
LCMS
TOC
FTIR
GCMS
UV
TM
LC
GC
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Selecting the Method
⚫ Selection of the best Method:
⚫ Element/-number
⚫ Concentration: major-, minor- or
trace elements
⚫ Sample preparation
⚫ Shimadzu Instruments:
⚫ RFA (EDX)
⚫ AAS (Flame/Furnace)
⚫ ICP-OES
⚫ ICP-MS
Se
ns
itiv
ity
0.000001
0.0005
0.005
0.05
0.5
50 Comparison of Detection limits
RFA
(mg/l)
ICP-
OES
Gra
ph
ite F
. -AA
S Fla
me
-
AA
S
ICPMS
12U. Oppermann/ K. Kartaschew | ICPMS | Food user meeting Bruxelles
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Methods
⚫ Beer Analysis⚫ MEBAK/EBC Methods for Cu, Mg, Al, Zn with AAS
⚫ MEBAK Method for Multi- Element Analysis with ICP-OES/MS
⚫ Water Analysis ⚫ DIN 38406- 6/-7/-8 Determination of Pb, Cu, Zn with AAS
⚫ DIN 38406-22 Determination of 22 Elements using ICP-OES
⚫ DIN EN ISO Determination of selected Elements using ICP-MS
⚫ Wine Analysis⚫ OIV-MA-AS323—07 Multi- Element Analysis with ICP-MS
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World Wine Production
MillionHektar
MillionHektoliter
Hektoliterpro Hektar
World 8 260 33
Europe 5 200 42
Asia 1.35 6
America 0.75 47 62
Africa 0.31 10
Ozeania 0.10 6
Germany 0.11 9 81
Croatia 0.03 1.4 46
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European Wine Regulation
Control Limits:
Aluminium8.00 mg/l
Arsenic 0.10 mg/l
Lead 0.25 mg/l
Boron 80 mg/l
Cadmium 0.01 mg/l
Copper 2.00 mg/l
Zinc 5.00 mg/l
Tin 1.00 mg/l
Trichloromethane 0.10 mg/l
Trichloroethene 0.10 mg/l
Tetrachloroethene 0.10 mg/l
Trichloromethane, Trichloroethene & Tetrachlorethene (total) 0.20 mg/l
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Copper/ Zinc
Concentration
• Metallic bitter taste > 1.0 mg/L
• Generate turbidity > 0.5 mg/L
• Copper oxidation > 0.5 mg/L
• Reducing the flavour >0.5 mg/L
• Influence on fermentation > 20 mg/L
Table 1: Influence of copper concentrations in wine
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Antimony?
Wine in PET- Bottles – Prof. Dr. Rainer Jung, University Rhein/Main
Languedoc Producer SKALLI in 2010: 2,5 Mio. PET bottles
http://blog.campus-geisenheim.de/index.php/2010/12/wein-aus-pet-flaschen-und-bechern-prof-dr-rainer-jung-im-interview-mit-dem-wiesbadener-kurier/
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Quantitative Analysis of Metals by AAS
Sequential in Flame- and Graphite furnace -Atomisation with AA-7000:Determination of Cu and Zn
http://www.shimadzu.eu/sites/default/files/Application_wine_SCA_120_026.pdf
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Sample Preparation
• Dilute with H2O 1:1• Alcohol Concentration ca. 5 %• HNO3 Concentration 0.1 %• Calibration Range: 0.005 to 50 mg/L.
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Quantitative Analyse of Metals
…using simultaneous ICP-OES: ICPE-9820
http://www.shimadzu.eu/sites/default/files/AN_SCA_115_023_Wine_0.pdf
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Quantitative Analysis of Metals
….with high sensitivity ICPMS-2030
http://www.shimadzu.eu/sites/default/files/AN_SCA_115_023_Wine_0.pdf
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ICP Coupled with Mass Spectrometry
Mini Torch
TechnologyMass Detector
Detection, Identification
and Quantitation of
Ionen
⚫ Analysis Technique: ⚫ Multi-Element Analysis : simultaneous as in ICP-OES⚫ Extreme Sensitivity => Analysis in Ultra- trace range (< ppb => ppt).
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Multielement Analysis in Wine
Table 1: ICPMS-2030 Results of Wine Sample [µg/L]
Table 2: Recovery rates
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Packaging: PET Bottles
⚫ Contamination by Sb2O3
⚫ Sb2O3 as Catalyst during PET Production
⚫ Start concentration Sb in PET bottle: 1,65 µg/l
⚫ EU limit exceeded after 30 days > 5 µg/l
⚫ At 40C after 4 days10 µg/l
Determination of Sb in alcoholic beverages, Schmitz, A. et al., Niederrhein University of applied Sciences, Krefeld, 2012
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Packaging: Glasbottles
⚫ Transmission/ Reflection of Glas
⚫ Sun protective glas with Fe (II)/ (III), Cu (II) oxide
⚫ UV-2600 with ISR-2600plus
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Chromium in Foodpackaging (1/2)
⚫ EU Packaging Directive 2014 (VerpackV)⚫ Limit values for Pb, Cd, Hg and Cr VI < 100 mg/kg
⚫ Speciation analysis using LC-ICPMS⚫ Toxicity of trace elements depends on concentration and oxidation state
⚫ Differentiation of Cr(III) and Cr(VI)
⚫ Cr(III) is not critical, Cr(VI) is toxic
⚫ Systemconfiguration⚫ ICPMS-2030
⚫ Prominence inert HPLC
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Chromium in Foodpackaging (2/2)
⚫ EU Packaging Directive 2014 (VerpackV)⚫ Limit values for Pb, Cd, Hg and Cr VI < 100 mg/kg
⚫ Calibration Curves⚫ Chrom III: 50, 100, 200, 500, 1000 ng/L
⚫ Chrom VI: 5, 10, 20, 50, 100 ng/L
⚫ Chromatograms of LC-ICPMS⚫ Overlay of Concentrations
⚫ Clear differentiation of Cr III & Cr VI
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Physical Testing
⚫ Bottle cork⚫ Wine- and Champaign bottles
⚫ Whisky bottles
⚫ Measurement⚫ Torque
⚫ Extraction force
⚫ ISO 9727-5:2007
⚫ Bottle sizes from 250 ml to 750 ml
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Sensoric Testing
⚫ Flavor/ Off flavor⚫ Natural flavor (exclusively from the fruit)
⚫ Synthetic flavors (not legal in fruit destillates)
⚫ Sensoric Quality control⚫ Color/ appearance
⚫ Smell
⚫ Taste
⚫ Testcriteria for Fruit Spirits
http://www.dlg-verbraucher.info/de/testergebnisse/spirituosen/regionales-im-trend-obstgeiste-und-braende.html
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Sensoric Testing
1: Color and appearence
2: Smell
3: Taste
Prof. Erich Leitner, Institute of Analytical Chemistry and Food Chemistry
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⚫ One of the best detectors: the human nose
Olfactometry for GCMS
Aroma Analysis
Substance Aroma Impression Threshold value [mg/L]
Ethanol alcoholic 100
Vanillin Vanilla 0.02
Hexanal fresh Gras 0.0045
Methylthiole rotten/ sour 0.00002
2,4,6-Tribromoanisol musty/ mouldy 0.00000002
20 pg/L (!!!)
Prof. Erich Leitner, Institute of Analytical Chemistry and Food Chemistry
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⚫ Enhanced selectivity: Triple-quadrupole technology
Aroma Analysis using GCMSMS
13.0 13.1 13.2 13.3 13.4 13.5 13.6 13.7 13.8 13.9 14.0
0.25
0.50
0.75
1.00
1.25
(x100,000)
2:210>195 TCA
1:215>197 TCA d5
13.0 13.1 13.2 13.3 13.4 13.5 13.6 13.7 13.8 13.9
0.25
0.50
0.75
1.00
1.25
1.50(x100,000)
2:210 TCA
1:215 TCA d5
Prof. Erich Leitner, Institute of Analytical Chemistry and Food Chemistry, TU Graz
GCMS-QP2020 GCMS-TQ8040
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Apple Spirit 1
Prof. Erich Leitner, Institute of Analytical Chemistry and Food Chemistry, TU Graz
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Apple Spirit 1 (Zoom)
Apple Spirit “Zoom”
1: Octan acid 4: 2-Methylbutyrate2: Terpineol 5: 1-Decanol3: Citronellol 6: Decane acid
Prof. Erich Leitner, Institute of Analytical Chemistry and Food Chemistry
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Conclusion
Shimadzu offers the full Productportfolio
and „taylor made“ solutions in
Quality control of Food and food packagings
for the highest level of food safety
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Questions/ noch Fragen/ avez-vous des questions?
Thank You!