AOAC-RI ERP Book - FAOM METHOD.pdf
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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