OMB First to Final Action Recommendation Checklist 11-12-18

3/9/2017

 Comprehensive technical conditions were used by 30 Labs

The comprehensive instrument, analyticalparameters and SPE cartridge of AOAC collaborative study

Technicalconditions

GC-MS (16 Labs)

GC-MS/MS(15 Labs)

LC-MS/MS (24 Labs)

5 types: Agilent; Waters; Thermo Fisher and Bruker 8 brands ： DB-1701;HP-5 ms; HP-5MSUI; HP-5MSI; DB-5MSUI; DB5-MS; BR-5ms; Rxi 5 Sil 3 Specification ： 30m×0.25mm×0.25μm; 15m×0.25mm×0.25μm; length20m/Diam. 0.180mm/Film 0.18µm 9 GC column temperature ： 40℃ hold 1 min , at 30℃/min to 130℃, at 5℃/min to 250℃, at 10℃/min to 300 ℃, hold 5 min 4 SPE cartridges ： CleanertTPT; InertSep GC/PSA; Agilent Technolongies BE Carbon 500mg/PSA; Envi Carb/PSA

12 types: Agilent; SHIMADZU; Waters and Thermo Fisher 14 brands ： ZORBAXSB-C18;phenomenex Luna C8; Waters Atlantis C18; phenomenex Luna C18 15 Specification ： 3.5 μm×100mm ×2.1mm; 3.5μm×150mm×2.1;150mm×2.00mm×3μm 11 GC column temperature : 0min-99%A, 3 min-70% A, 6 min-60% A, 9 min- 60%A, 15 min -40% A, 19 min -1% A, 23 min -1% A, 23.01 min -99% A 5 SPE cartridges ： CleanertTPT; InertSep GC/PSA; Agilent Technolongies BE Carbon 500mg/PSA; Envi- Carb; Envi Carb/PSA

Instrument （ 22 ）

5 types: Agilent; Varian

5 brands ： DB-1701;Restek Rtx 1701; MR2; HP-5 ms; HP-5MSUI

Chromatographic column （ 27 ）

Specification （ 19 ）

30m×0.25mm×0.25μm

① GCcolumn temperature (14) ② LCgradient program(11)

5 GC column temperature ： 40℃ hold 1 min , at 30℃/min to 130℃, at 5℃/min to 250℃, at 10℃/min to 300 ℃, hold 5 min 3 SPE cartridges ： CleanertTPT; UCT (ECPSACB506); Envicarb/PSA

SPE cartridge(12)

30

27

22

19

20

14

11

11

10

0

Instrument

GC/LC column Column specification

GC column temperature

LC gradient program SPE cartridge

 30 laboratories have submitted to SD clusters of data totaling 81315 the method efficiency can be evaluated comprehensively with these five classes of data, and errors can be analyzed and traced. In addition, it also includes a 5000-page of raw data reports and chromatographs.

10000 15000 20000 25000 30000 35000 40000 45000

40586

Five types of data

22879

8915

6742

2193

0 5000

Results of target pesticides

Monitoring ions

Ion abundance

Calibration curve

Results of pre- collaborative study

A lot of outliers obtained by one out of 30 laboratories were eliminated because of its digression from the operation protocol, so this laboratory’s data was excluded from the evaluation of the method that ensued.

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