气相色谱-串联质谱法测定半边莲中九种农药残留

Determination of nine pesticide residues in banbianlian by gas chromatography-tandem mass spectrometry

建立了一种测定半边莲中α-六六六等九种有机氯农药的气相色谱-串联质谱方法。样品用醋酸-乙腈提取、固相萃取净化后,气相色谱-串联质谱测定,采用5%苯基甲基聚硅氧烷为固定液的弹性石英毛细管柱(0.25 mm×30 m,0.25μm)为色谱柱,载气为高纯氦气,多反应监测模式检测9种有机氯农药残留。结果表明,9种目标农药在10~400μg·L-1线性良好,相关系数均大于0.995,方法检出限为0.57~4.3μg·L-1,定量限为1.9~14μg·L-1,方法平均回收率为64.22%~121.4%,相对标准偏差为3.41%~13.3%。所测定的53批半边莲样品中9种有机氯残留均远低于《中国药典》2015年版规定要求。本实验所建立的方法能满足半边莲中9种目标农药残留的分析要求。

A method of gas chromatography-tandem mass spectrometry was established for the determination of nine organochlorine pesticides in Banbianlian.The samples were extracted by acetic acid-acetonitrile and purified by solid phase extraction,and then determined by gas chromatography-tandem mass spectrometry.The elastic quartz capillary column(0.25mm×30m,0.25μm)with 5%phenylmethyl polysiloxane as solid phase was used as the chromatographic column,and the carrier gas was high purity helium gas.The residues of nine organochlorine pesticides were detected by multi-reaction monitoring mode.The results indicated that calibration curves of nine target pesticides were linear in the range of 10~400μg·L-1 with correlation coefficient larger than 0.995.The limits of detection ranged from 0.57 to 4.3μg·L-1 and the limits of quantification ranged from 1.9 to 14μg·L-1.The average recoveries of the method were 64.22%~121.4%with relative standard deviations ranged from 3.41%to 13.3%.The residues of nine organochlorine in the 53 batches Banbianlian were far below the limits of the 2015 Chinese Pharmacopoeia.The established method in current experiment meets the requirements for the detection of nine organochlorine pesticides in Banbianlian.