GC-MSMS同时测定杭白菊中68种农药残留.pdfVIP

GC-MS/MS 同时测定杭白菊中 68 种农药残留  * 朱海花，徐强，冯瑛，王溶溶(浙江省中药研究所有限公司，杭州 310023) 摘要：目的 采用GC-MS/MS 建立同时测定杭白菊中68 种农药残留的分析方法。方法 样品采用QuEChERS 前处理程 序，经 1%冰醋酸浸泡30 min 后，乙腈提取，经装有无水硫酸镁900 mg 、PSA 300 mg 、十八烷基键合硅胶300 mg 、硅胶 300 mg 和石墨化炭黑90 mg 的分散固相萃取净化管净化，采用GC-MS/MS 动态多反应监测模式，进行定性定量分析。结 果 68 种农药在各自浓度范围内线性关系良好，相关系数r 均0.993 。在20 ，100，200 μg·kg1 3 个不同加标水平下，除 六氯苯、甲基五氯苯硫醚、苯氟磺胺、p,p -滴滴伊和氯氟氰菊酯外，大部分农药的回收率均在70.0%~120.0%之间，RSD 在0.4%~13.9%之间。方法的检出限为0.2~25.6 μg·kg1 ，定量限为0.8~85.5 μg·kg1。结论 该方法简单、快速、高效、 灵敏，可为杭白菊中多农药残留的快速筛查和测定提供一种有效的分析手段。 关键词：杭白菊；农药残留；气相色谱-三重四极杆串联质谱；QuEChERS 中图分类号：R917 文献标志码：B 文章编号：1007-7693(2018)11-1702-07 DOI: 10.13748/ki.issn1007-7693.2018.11.024 引用本文：朱海花, 徐强, 冯瑛, 等. GC-MS/MS 同时测定杭白菊中68 种农药残留[J]. 中国现代应用药学, 2018, 35(11): 1702-1708. Simultaneous Determination of 68 Pesticide Residues in Chrysanthemum Morifolium by GC-MS/MS * ZHU Haihua, XU Qiang, FENG Ying, WANG Rongrong (Zhejiang Research Institute of Traditional Chinese Medicine Co., Ltd., Hangzhou 310023, China) ABSTRACT: OBJECTIVE To establish a multi-residue analytical method for the determination of 68 pesticides in Chrysanthemum morifolium by GC-triple quadrupole mass spectrometry(GC-MS/MS). METHODS Samples were treated with QuEChERS pretreatment method. They were extracted with acetonitrile after soaking in 1% acetic acid for 30 min, and then purified by dispersed solid-phase extraction and purification tubes containing 900 mg of anhydrous magnesium sulfate, 300 mg of PSA, 300 mg of octadecyl-bonded silica, 300 mg of silica gel and 90 mg of graphitized carbon black. The GC-MS/MS dynamic multiple reaction monitoring (dMRM) mode was used for the