GC-MS/MS测定何首乌中100种农药多残留

Determination of Residues of 100 Pesticides in Polygoni Multiflori Radix by GC-MS/MS

目的:建立何首乌中100种农药的气相色谱-质谱法(GC-MS/MS)测定方法,并采用此方法对53批何首乌(包括43批生品和10批制品)样品进行农药初步筛查。方法:样品经乙腈高速匀浆提取,浓缩后加分析保护剂,采用GC-MS/MS进行测定。质谱以动态多反应监测模式(MRM)采集数据,采用空白基质匹配-分析保护剂标液进行定量计算,在提高响应值的同时改善了峰形。结果:100种农药线性关系良好,r均大于0.99,加标回收率试验中100种农药(113个单体)的回收率为70.4%~107.4%,RSD均小于11.40%,符合痕量测定的要求。检测的53批何首乌样品中均未检测到本方法涉及的农药,初步表明何首乌农药残留引起的风险较小。结论:此方法检测指标基本包括GC-MS/MS可测定的大多数禁用农药,方法灵敏度高、准确性好,可用于何首乌中农药残留的筛查检测,同时为基质类似中药材的农药残留检测方法提供参考。

Objective:To establish a gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the determination of 100 pesticides in Polygoni Multiflori Radix,and to use this method to detect pesticides in 53 batches of samples(10 batches of Polygoni Multiflori Radix Praeparata and 43 batches of raw products).Methods:The sample were respectively mixed with acetonitrile,extracted by high speed homogenizer,concentrated,and added with analyte protectant before GC-MS/MS analysis.For the MS,multiple reaction monitoring(MRM)was applied to collect data,and blank matrix matching-analyte protectant standard method was used for quantitative analysis to increase the accuracy and improve the peak shape.Results:The calibration curves of all targets showed good linearity with correlation coefficients>0.99.The average recoveries for all target compounds ranged from 70.4%to 107.4%,with relative standard deviations<11.40%,which met the requirements of trace determination.A total of 53 batches of samples were determined and the results showed that no pesticide was detected in them.This indicated that the risk caused by pesticide residues in Polygoni Multiflori Radix was low.Conclusion:This method is applicable to most of the banned pesticides,which is highly sensitive with high accuracy.It can be employed to the screen and detect pesticide residues in Polygoni Multiflori Radix and can serve as a reference for the detection of pesticide residues with matrix similar to Chinese medicinal material.