GC-MS法测定金银花中12种有机磷农药的残留量

Determination the 12 Kinds of Phosphate Pesticides in Honeysuckle by Gas Chromatography-Mass Spectrometry

目的:建立金银花中12种有机磷农药残留量的测定方法。方法:样品以丙酮超声提取,并采用凝胶渗透色谱(GPC)和氨基固相萃取柱(NH_2-SPE)结合的方法进行净化,选用气相色谱与质谱串联技术(GC-MS)在DB-5MS毛细管柱上用程序升温技术分离,采用选择离子检测方式,以保留时间和特征离子进行目标成分的定性鉴别,外标法对样品进行测定。结果:12种有机磷农药在50～1000μg·L^(-1)范围内呈良好的线性关系,12种农药的方法定量限在3.6～7.2μg·kg^(-1)之间,三个水平添加回收率在72.21%～107.72%,RSD<10%(n=9)。结论:本方法灵敏度高,重复性好,可用于金银花中12种有机磷农药残留的检测。

Objective ： To establish an analytical method for the simultaneously determination of 24 pesticide residues in Honeysuck- le. Method： The sample was extracted with acetone,and the extract was cleaned using GPC and SPE,The eluate was concentrated under nitrogen blowing. Based on GC-MS, the pesticides were separated with a DB-5MS column using a temperature program and were detected with a mass selective detector in selective ion monitoring （SIM） mode. The target pesticides were identified by comparing their retention times and characteristic ions with reference. Result： The linearity of the method was good within 50-1 0001μg·L-1, and all the limits of quantification （LOQs） were within 3.6 and 7. 2μg·kg-1. The average spiked recoveries in three levels were 72. 21%-107.72% with RSD below 10% （n = 9）. Conclusion： The method is sensitive for the residue analysis of 12 phosphate pesticide in Honeysuckle.