液相色谱-串联质谱法测定枸杞中氨基甲酸酯类农药残留量

建立了同时测定枸杞中涕灭威亚砜、涕灭威砜、灭多威、3-羟基克百威、涕灭威、克百威、抗蚜威、甲萘威8种氨基甲酸酯类农药残留的液相色谱-串联质谱(LC-MS/MS)检测方法.枸杞样品经乙腈提取,Carbon/NH2小柱净化,C18柱分离后,在电喷雾正离子化模式下,于三重四极杆质谱仪上以多反应监测方式测定.结果表明:8种农药...

Determination of 8 Carbamate Pesticide Residues in Lycium by Liquid Chromatography-Tandem Mass Spectrometry

A liquid chromatography-tandem mass spectrometric(LC-MS/MS)method was developed for simultaneous determination of aldicarb-sulfoxide,aldicarb-sulfone,methomyl,carbofuran-3-hydroxy,aldicarb,carbofuran,pirimicarb and carbaryl carbamates pesticides in Lycium.The sample was extracted with acetonitrile,and then cleaned up by Carbon/NH2 cartridge.8 pesticides were separated on a C18 column using 2 mmol/L ammonium acetate(A)-acetonitrile(B) as mobile phase in gradient elution.The analytes were detected with positive-ion electrospray ionization-mass spectrometry in MRM mode.Under the optimal conditions,the calibration curve was linear in the range of 20-500 μg/L and the detection limit(S/N=3)ranged from 0.01 to 5 μg/kg.The results showed that the mean recoveries of 8 pesticides at three spiked concentration levels of 0.02,0.05 and 0.1 mg/kg were in the range of 77.7%-98.6%,85.0%-103.8% and 76.8%-102.2%,respectively,with relative standard deviations(RSDs) of 2.48%-9.98%,4.14%-10.40% and 8.33%-18.80%,respectively.The method is rapid,sensitive and reliable,suitable for analyzing carbamate pesticide residues in Lycium.