Citation: YANG Xin, LI Peng, MIAO Hong, ZHAO Yunfeng, WU Yongning. Determination of N-methyl carbamate pesticides in diet samples by high performance liquid chromatography-linear ion trap mass spectrometry with gel permeation chromatography cleanup[J]. Chinese Journal of Chromatography, ;2014, 32(5): 499-505. doi: 10.3724/SP.J.1123.2013.12041 shu

Determination of N-methyl carbamate pesticides in diet samples by high performance liquid chromatography-linear ion trap mass spectrometry with gel permeation chromatography cleanup

YANG Xin ^1,, ,
LI Peng ^1,2 ,
MIAO Hong ^1,2 ,
ZHAO Yunfeng ^1,2 ,
WU Yongning ^1,2

1.
1. China National Center for Food Safety Risk Assessment, Beijing 100021, China;

Corresponding author: YANG Xin,
Received Date: 31 December 2013
Available Online: 26 March 2014
Fund Project: “十二五”国家科技支撑计划项目(2011BAK10B06). (2011BAK10B06)

A method for the determination of N-methyl carbamate (NMC) pesticides in diet samples was developed by high performance liquid chromatography-linear ion trap mass spectrometry (HPLC-LIT-MS). The samples with the isotope internal standard were ultrasonically extracted with acetonitrile saturated with cyclohexane, and then cleaned-up by passing through gel permeation chromatographic (GPC) column. The LC separation was performed on a CAPCELL PAK CR column (100 mm×2.1 mm, 5 μm; SCX-C₁₈ (1:4)) using acetonitrile and 5 mmol/L ammonium formate/0.1% (v/v) formic acid aqueous solution as mobile phases (gradient elution) at a flow rate of 0.2 mL/min. The ionization of the analytes was performed by positive electrospray mode. Selective reaction monitoring (SRM) was used for the monitoring of MS³ transitions for each compound. The internal standard was used for quantitation. The average recoveries were in the range of 60.4%-114%, and the relative standard deviations (RSDs) were all not more than 16.2%. The limits of detection (LODs) were 0.001-0.010 mg/kg. The method was successfully applied to the determination of 15 compounds of interest in nine foodstuffs from the fourth Chinese Total Diet Study (TDS) performed in 2007, and aldicarb and carbofuran were found in several samples.
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