食糧　その科学と技術　No.46( )

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1 , IARC A ppb ppm, WHOµg/L GC GC GCMS GC MS, d

2 O O O NH 2 Br 2 NEt 3 Br NH 2 NH 2 Br Br GC, [C H NO Br] + m/z [C H NO Br] m/z SIM [C H D NO Br] m/z [C H D NO Br] + m/z Br Br HBr [C H NO Br] + m/z GC -d [C H NO Br] + m/z [C H D NO Br] + m/z [C H NO Br] + m/z [C H D NO Br] + m/z C C HBr GC MS GC GC MS LC MS/MS,,,, LCMS/MS GCMS LCMS/MS LC MS/MS ODS

3 C electrospray ionization, ESI[MH] + m/z m/z ///selected reaction monitoring, SRMm/z GCMS d C m/z LCMS LCSIMMS/MS SRM GCMSLC MS/MS EC Directorate General Joint Research CentreDG JRC HEATOX DG JRCInstitute for Reference Materials and Measurements IRMMHEATOX EU DG JRC Central Science Laboratory CSL, Swedish National Food Administration SNFA, the Nordic Committee on Food Analysis NMKL ISO IUPAC Protocol for the Design, Conduct and Interpretation of MethodPerformance Studies LCMS/MSGCMS GCMS IRMM

4 Standard Operating Procedure, SOP LC MS/MS IRMM IRMM

5 TEST SAMPLES FOR CHEMICAL ANALYSIS gl

6 2g 5-13 C 3 400ng200 L 1:13mL 20 ml 15 3,000 g 5 10 ml ml 8 ml 15 3,000 g 5 4 ml 0.5 g mL L GC-MS 50%-phenyl-50%-polymethylsilicone0.25 mm i.d. 30 m, 0.25 mm 1 ml/min : min20 /min175 5 min20 /min280 5 min 280 EI+70 ev SIM m/z 106, 133, 135, 149, 151, 152, 154

7 2g 10 ml 40 ml -d ng Isolute Multimode Isolute ENV+ 4 ml 60% 2 ml 500 L 10 L LC-MS/MS Hypercarb 0.1% 400 L/min SRM m/z 72 > 55, 72 > 54, 72 > 44, 75 > 58 ng,ng ml GCMS GCMS HBr

8 C d MS HD C ml ml ml ml g g ml E GCMSm/z m/z GCMS

9 GC MS GC MS GCMS GCMS m/z,, Journal of Chromatography A EU EU LCMS/MS GCMS blind duplicate study

10 g LC MS/MS LC MS/MSMandels h Mandels h Mandels h Mandels k, Cochrans test, Grubbs test LCMS/MS *LCMS/MS ERM BD A Horwitz g/kgermbd g/kg LC MS/MS GCMS HBr

11 A B A A ERM-BD B B C LCMS/MS RSDr RSD R g/kg% % Ho r Ho R g/kg GCMS RSD r RSD R % % Ho r Ho R * * * * * * * * RSDrRSD R Ho r HorRat *RSD r RSD R RSD R RSD r Mandel's h Participant

12 Participant Blank - white bread crumb Blank - mashed potato powder Butter biscuits A Toasted bread Butter biscuits B Spiced biscuits potato crisps A g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ * * Participant Spiked mashed potato powder Commercial Potato crisps A Crispbread CRM; g / kg potato crisps B Commercial Potato crisps B potato crisps C g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg * * <LOD <LOQ *

13 Participant Blank white bread crumb Blank mashed potato powder Butter biscuits A Toasted bread Butter biscuits B Spiced biscuits potato crisps A g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Participant Spiked mashed potato powder Commercial Potato crisps A Crispbread (CRM; g / kg potato crisps B Commercial Potato crisps B potato crisps C g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg g/kg nq <LOQ nq < LOD< LOQ nq LC MS/MSLCMS/MSGCMS GC MS LCMS/MS GC MS GCMS GC MS LC

14 MS/MS GCMS GC MS GCMS LC MS/MS GCMS,. Rosén, J. and Hellenäs, K., Analysis of acrylamide in cooked foods by liquid chromatography tandem mass spectrometry. The Analyst,,. Tareke, E., Rydberg, P., Karlsson, P., Eriksson, S. and Törnqvist, M., Analysis of acrylamide, a carcinogen formed in heated foodstuffs. J. Agric. Food Chem.,,. pp..,. Wenzl, T., Beatriz de la Calle, M. and Anklam, E., Analytical methods for the determination of acrylamide in food products: a review, Food Addit. Contam.,,

15 . Horwitz, W., Protocol for the design, conduct and interpretation of method performance studies. Pure & Appl. Chem.,,. Wenzl, T., Karasek, L., Rosen, J., Hellenaes, K., Crews, C., Castle, L., and Anklam. E., Collaborative trial validation study of two methods, one based on high performance liquid chromatographytandem mass spectrometry and on gas chromatographymass spectrometry for the determination of acrylamide in bakery and potato products. J. Chromatography A,,.

☆H23 13－農薬一斉分析（大垣）.doc

☆H23 13－農薬一斉分析（大垣）.doc 13 56 2011 Examination of Determination of Residual Pesticides in Agricultural Products Yuki OHGAKI, Katsuhiro HAYASHI, Hiroyuki KAWAI, and Kyoko SHIMURA GC/MS 92 LC/MS/MS 60 150 n- 5 GC/MS 92 79 70% LC/MS/MS

食糧 その科学と技術 No.46( )

食糧　その科学と技術　No.46( )