气相色谱-三重四级杆串联质谱法测定易腐果蔬中的环酰菌胺残留量

Determination of Fenhexamid Residues in Fruits and Vegetables by GC-MS/MS

本文建立了易腐果蔬中环酰菌胺的气相色谱-三重四级杆串联质谱检测方法。将试样中残留的环酰菌胺用乙腈提取,经氯化钠盐析分层,提取液经无水硫酸镁、PSA吸附剂和C_(18)固相吸附剂分散固相萃取净化,气相色谱-三重四级杆串联质谱仪GC-MS/MS确证,外标法定量。方法通过空白基质溶液稀释标准物质建立校正曲线,以消除基质效应。结果表明,环酰菌胺在0.01~0.5 mg/L范围内具有良好的线性关系,相关系数在0.9998以上;在0.02~1.0 mg/kg范围内,平均添加回收率在88.83%~98.50%之间,相对标准偏差在2.5%~5.5%之间。该方法的定量限为0.01 mg/kg。

A gas chromatography-triple quadrupole mass spectrometry method was established to determine fenhexamid residue in perishable vegetables and fruits.Analytes were extracted from samples using acetonitrile,and then purified by solid phase extraction cartridge packaged with sorbent primary secondary amine(PSA)and C_(18).The residue was determined by GC-MS/MS using external standard method,and the interference of matrix was deducted by the matrix-matched calibration standards curve.A good linearity of calibration curve was exhibited over a concentration range of 0.01 mg/L to 0.5 mg/L for fenhexamid with a correlation coefficient above 0.9998.Average recoveries for fenhexamid in 5 samples at spiked levels of 0.02-1.0 mg/kg was between 88.83%and 98.50%,with a relative standard deviations between 2.5%and 5.5%.For fenhexamid,the limit of detection was 0.01 mg/kg.