竹笋中40种农药残留的固相萃取/气相色谱-质谱法同时测定

Simultaneous Determination of 40 Pesticides Residue in Bamboo Shoots by GC-MS Method with Solid Phase Extraction

建立了竹笋中40种农药（包括有机磷类、有机氯类、氨基甲酸酯类、拟除虫菊酯类、三唑类和杂环类）残留的同时检测方法。样品以乙腈为提取溶剂，高速匀浆提取，经PSA固相萃取小柱净化，利用GC—MS／SIM进行测定。结果表明，40种农药在一定质量浓度范围内线性良好，相关系数为0．9946～0．9998。在0．050—2．0mg／kg范围内的加标回收率为68％～119％，相对标准偏差为1．1％～20．0％，方法的定量下限（S／N：10）为0．01～0．05rag／kg。该方法简便快速、准确可靠，适用于竹笋中农药多残留的同时检测。

A muhiresidue analytical method was developed for the simultaneous determination of 40 pesticide residues in bamboo shoots based on solid phase extraction（SPE） coupled with gas chromatography- mass spectrometry （GC -MS）. The pesticide residues in bamboo shoots were extracted with acetonitrile by homogenate extraction technology, concentrated after salting out. The extract was cleaned up on a solid phase extraction column with 500 mg primary secondary amine （PSA） , eluted with acetone. The eluate was evaporated to near dryness and redissolved with n-hexane. The analytes were confirmed and determined by GC -MS under selected ion monitoring mode. The results showed that the calibration curves of 40 pesticide residues were linear in the certain concentration range with correlation coefficients of 0. 994 6 - 0. 999 8. The average recoveries at three spiked levels were in the range of 68% -119% with relative standard deviations（RSDs） of 1.1% -20. 0% . The limits of quantitation（LOQs, S/N = 10） of 40 residues were in the range of 0. 01 -0. 05 mg/kg. The proposed method was sensitive and reliable for the determination of 40 pesticide residues in bamboo shoots.