GC-MS/MS检测陈皮药材中179种农药残留

Determination of 179 Pesticides in Citri Reticulatae Pericarpium by GC-MS/MS

目的：基于气相色谱-串联质谱联用技术,建立GC-MS/MS农药多残留筛查与检测方法;在满足农药残留量检测方法学考察的技术要求基础上,对陈皮中179种农药残留量进行筛查与检测,全面了解陈皮种植过程中农药使用情况,以及陈皮药材的农药残留量。方法：陈皮样品先经2次乙腈匀浆提取,过固相萃取柱（SPE）净化,浓缩,滤过,加内标分析保护剂,采用GC-MS/MS技术进行检测。结果：建立了179种禁用、限用、高毒、国内常用农药指标的GC-MS/MS测定法;针对陈皮基质,建立了满足方法学要求的提取、净化、测定方法,该提取净化方法回收率在60%~120%,RSD≤15%,方法检出限总体在0.01 mg·kg^-1以下。结论：建立的农药多残留方法指标较全面,有针对性,且方法灵敏度高,准确性好,可广泛地筛查与检测陈皮中农药多残留量,从而全面地反映农药污染情况;筛查结果表明,陈皮种植中农药使用种类较多,农药残留污染情况比较严重,陈皮药材的使用存在农药残留量超标风险。

Objective： To establish a GC-MS/MS method for detecting 179 pesticides in Citri Reticulatae Pericarpium,in order to find out the current situations of pesticide residues in Citri Reticulatae Pericarpium.Method： The samples were extracted with acetone for twice,cleaned up by solid-phase extraction（SPE）,concentrated,filtered,added with internal standard analysis protection agent,and then determined by GC-MS/MS.Result： The method of GC-MS/MS was established for determining 179 pesticides,including forbidden,limited,high-toxic and common pesticides. The recoveries of most pesticides ranged from 60% to 120%,with RSDs less than 15%. The limits of determination were below 0. 01 mg·kg^-1. Conclusion： This method is sensitive and accurate,and can be used for the determination of multi-residual pesticides in Citri Reticulatae Pericarpium. The findings show that many finds of pesticides were used in planting oranges,which causes serious pesticide residues pollution. Therefore,there is a risk of using Citri Reticulatae Pericarpium with excessive pesticide residues.