5. AOACSPDSMethods-2018AwardsV3

68

Peak area ratio = peak area of analyte/peak area of IS

Table 2017.11I. Valco valve schedule Time, min Position

Destination

( b ) Calculation of the unknown samples .—Calculate the peak area ratio of unknown samples. ( c ) Determination of unknown samples .—( 1 ) Compare the peak area ratio of unknown sample and the MRL. ( 2 ) When peak area ratio of each peptide from unknown sample is less than from MRL, the result is not confirmed presence. When peak area ratio of each peptide from unknown sample is more than from MRL, the result is positive. ( 3 ) When all three peptides of each protein have positive results, the protein is confirmed presence. Otherwise, the protein is not confirmed presence. References: J. AOAC Int . (future issue) AOAC SMPR 2016.016 J. AOAC Int . 100 , 292(2017) DOI: 10.5740/jaoacint.2016.016 Posted: February 2018

0 1 9

A B A

Waste

MS analysis

Waste

Table 2017.11J. Instrument settings Fixed Ion transfer voltage IS

5500

Probe temperature Interface heater

TEM

500

ihe

On

Typical

Curtain gas

CUR GS1 GS2 CAD

20 40 50

Ion source gas 1 Ion source gas 2

Collision gas

High

Table 2017.11K. Analytes

Common name

Protein analytes

Species

Protein

Cas-1, Cas-2, Cas-3 Lac-1, Lac-2, Lac-3

Cow (milk) α-S1-casein Cow (milk) β-Lactoglobulin

Bos taurus Bos taurus Oryza sativa Pisum sativum Glycine max

Glu-1, Glu-2

Rice Pea Soy

Glutelin

Vic-1, Vic-2, Vic-3 Gly-1, Gly-2, Gly-3

Vicilin

Glycinin G1

Table 2017.11L. Transition parameters Protein analyte Peptide Q1 a

Q3 b

CE c

Cas-1 Cas-2 Cas-3

FFVAPFPEVFGK

692.9 920.5 29 634.4 991.6 33

YLGYLEQLLR

HQGLPQEVLNENLLR 880.5 1324.7 51 Lac-1 VYVEELKPTPEGDLEILLQK 1157.1 1453 60 Lac-2 VLVLDTDYK 533.3 853.5 23 Lac-3 LIVTQTMK 467.3 707.4 21 Glu-1 EGSLLLPHYNSR 693.4 773.6 40 Glu-2 GDFELVGQR 510.8 572.5 26 Vic-1 ALPNDVLANAYR 658.9 566.8 26 Vic-2 LQAFEPIR 487.3 732.5 23 Vic-3 GDEFGAFTPIQYK 736.9 1024.8 33 Gly-1 VLIVPQNFVVAAR 713.4 1001.6 33 Gly-2 VFDGELQEGR 575.3 903.4 29 Gly-3 LNALKPDNR 520.8 629.3 32

a  Selected mass in quadrupole 1 (Q1). b  Selected mass in quadrupole 3 (Q3). c  Collision energy (CE).

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