Citation: LIU Xiaoqin, TONG Ling, MENG Wenting, SUN Guoxiang. Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(8): 869-877. doi: 10.3724/SP.J.1123.2015.04005 shu

Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry

1.
1. School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China;

Corresponding author: SUN Guoxiang,
Received Date: 3 April 2015

Fund Project: 国家"重大新药创制"科技重大专项(2013ZX09402202). (2013ZX09402202)

A method was established for the simultaneous determination of 99 pesticide residues with combination of solid-phase extraction technique (SPE) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS). The sample was extracted with ethyl acetate, and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0.001-0.25 mg/L, with correlation coefficients (r²) > 0.99. The limits of quantification (LOQs) were between 0.001-0.050 mg/kg. The recoveries were between 66.7% and 128.0% with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg/kg. This method has been applied to determine thirteen batches of commercially available samples, chlorpyriphos-ethyl and p,p'-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate, reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.
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沈阳化工大学材料科学与工程学院沈阳 110142