, IARC A ppb ppm, WHOµg/L GC GC GCMS GC MS, d
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
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
Standard Operating Procedure, SOP LC MS/MS IRMM IRMM
TEST SAMPLES FOR CHEMICAL ANALYSIS gl
2g 5-13 C 3 400ng200 L 1:13mL 20 ml 15 3,000 g 5 10 ml 41 15 ml 8 ml 15 3,000 g 5 4 ml 0.5 g 15 0.5mL 40 50 L GC-MS 50%-phenyl-50%-polymethylsilicone0.25 mm i.d. 30 m, 0.25 mm 1 ml/min 250 15:1 40 1 min20 /min175 5 min20 /min280 5 min 280 EI+70 ev SIM m/z 106, 133, 135, 149, 151, 152, 154
2g 10 ml 40 ml -d 3 400 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
C d MS HD C ml ml ml ml g g ml E GCMSm/z m/z GCMS
GC MS GC MS GCMS GCMS m/z,, Journal of Chromatography A EU EU LCMS/MS GCMS blind duplicate study
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
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
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 *
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
MS/MS GCMS GC MS GCMS LC MS/MS GCMS,. http://aa.iacfc.affrc.go.jp. 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.,,
. 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,,.