LC-MS/MS测定川牛膝中57种农药残留及风险评估

目的：采用液相色谱串联质谱法（LC-MS/MS）建立川牛膝中57种农药的测定方法，并采用此方法对348批川牛膝样品进行农药筛查。方法：样品经乙腈提取，分散固相萃取QuEChERS净化，采用LC-MS/MS进行测定，多反应监测模式采集数据，基质匹配外标法定量，采用点评估法对检出结果进行风险评估分析。结果：57种农药线性关系良好，r均大于0.996,57种农药的平均加样回收率为62.5%～113.3%,RSD%均小于10%。348批川牛膝中检出20种农药，其中有4种禁用农药（均未超出限量规定）、6种植物生长调节剂、10种常用农药；风险评估结果显示，川牛膝中农药残留风险较低，植物生长调节剂使用较普遍。结论：该方法简便、灵敏、准确，适用于川牛膝中多农药残留的快速筛查与检测，可为川牛膝的农药风险评估和规范化种植提供数据参考。

Determination and Risk Assessment of 57 Pesticide Residues in Cyathulae Radix by LC-MS/MS

Objective To establish a method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determining 57 pesticide residues in Cyathulae Radix and use this method to detect pesticide residues in 348 batches of Cyathulae Radix samples.Methods The samples were extracted with acetonitrile. The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERs) method was employed to purify the extract, which was then determined by LC-MS/MS. Multiple reaction monitoring (MRM) was adopted to collect data, and the matrix-matched standard curve was established for quantitation. The risk assessment was carried out with the deterministic approach.Results The calibration curves of all targets showed good linearity with correlation coefficients>0.996. The average recoveries for all target compounds ranged from 62.5% to 113.3%, with relative standard deviations<10.0%. Twenty pesticides were detected in 348 batches of samples, including 4 banned pesticides, 6 plant growth regulators, and 10 common pesticides. Risk assessment results showed that the risk of pesticide residues in Cyathulae Radix was low, and plant growth regulators were commonly used.Conclusion The established method is simple, sensitive, and accurate and can be used for the rapid screening and detection of multiple pesticide residues in Cyathulae Radix. The findings provide a reference for the pesticide risk assessment and standardized planting of Cyathula officinalis Kuan.