GC-MS/MS检测陈皮药材中179种农药残留

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。

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

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.