气相色谱-串联质谱法同时检测梨中34种农药残留量

Simultaneous determination of 34 kinds of pesticide residues in pears by gas chromatography-tandem mass spectrometry

目的建立气相色谱-串联质谱法同时检测梨中34种农药残留量(包括有机磷、有机氯和拟除虫菊酯类农药)的方法。方法匀浆后的样品经乙腈(含1%乙酸)溶液提取,N-丙基乙二胺(primary secondary amine,PSA)净化,无水硫酸镁脱水,氮吹浓缩后,采用气相色谱-串联质谱多反应离子监测(multi reaction monitor,MRM)方法检测,外标法定量。结果 34种农药在0.001~0.1μg/m L的线性范围内均呈现良好的线性关系(r2为0.9973~0.9993)。0.01、0.10 mg/kg加标浓度下,各农药的平均回收率为83.3%~109.4%,相对标准偏差为1.3%~10.8%,该方法定量限为5.0μg/kg。结论该方法灵敏度高,准确性好,简便快速,适用于梨中多种农药残留量的检测。

Objective To establish a method for the simultaneous determination of 34 kinds of pesticide residues in pears by gas chromatography-tandem mass spectrometry. Methods The samples were extracted by acetonitrile （containing 1% acetic acid） solution, purified by primary secondary amine （PSA） and dehydrated by Magnesium sulfate anhydrous, and then detected by gas chromatography-tandem mass spectrometry with the method of multi reaction monitor （MRM）, quantified by the external standard method. Results The 34 kinds of pesticides showed good linear relationships in the linear range of 0.0010-0.1 μg/mL （r^2 were 0.9973-0.9993）. The average recoveries of pesticides at spikes of 0.01 and 0.10 mg/kg were 83.3%-109.4%, and the relative standard deviations were 1.3%-10.8%. The limits of quantification were 5.0 μg/kg. Conclusion The method is simple, rapid, and has high sensitivity and good accuracy, which is suitable for detecting a plurality of pesticide residues in pears.