LC-MS/MS法测定川牛膝中57种农药残留及风险评估
投稿时间:2023-02-06  修订日期:2023-02-10   点此下载全文
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作者中文名作者英文名单位中文名单位英文名E-Mail
何成军 He Cheng-jun 四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室 Sichuan Provincial Institute for Drug Control/NMAP Key Laboratory of Quality Evaluation of Chinese Patent Medicine (Traditional Chinese Patent Medicine) heye1217@163.com 
王莹 WANG Ying 中国食品药品检定研究院 National Institutes for Food and Drug Control wayi_1986@ 163.com 
耿昭 GENG Zhao 四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室 Sichuan Provincial Institute for Drug Control/NMAP Key Laboratory of Quality Evaluation of Chinese Patent Medicine (Traditional Chinese Patent Medicine) gengzhao713@hotmail.com 
钟恋 ZHONG Lian 四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室 Sichuan Provincial Institute for Drug Control/NMAP Key Laboratory of Quality Evaluation of Chinese Patent Medicine (Traditional Chinese Patent Medicine) zhonglian3678@126.com 
高必兴 GAO Bi-xing 四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室 Sichuan Provincial Institute for Drug Control/NMAP Key Laboratory of Quality Evaluation of Chinese Patent Medicine (Traditional Chinese Patent Medicine) laughgao@foxmail.com 
金红宇 JIN Hong-yu 中国食品药品检定研究院 National Institutes for Food and Drug Control jhyw@nifdc.org.cn 
杨蕾 YANG Lei 四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室 Sichuan Provincial Institute for Drug Control/NMAP Key Laboratory of Quality Evaluation of Chinese Patent Medicine (Traditional Chinese Patent Medicine) 1504868330@qq.com 
马双成 MA Shuang-cheng 中国食品药品检定研究院 National Institutes for Food and Drug Control masc@nifdc.org.cn 
苟琰* GOU Yan 四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室 Sichuan Provincial Institute for Drug Control/NMAP Key Laboratory of Quality Evaluation of Chinese Patent Medicine (Traditional Chinese Patent Medicine) gouyan0101@hotmail.com 
基金项目:四川省药品监督管理局科技计划项目(编号:2021002);四川省药品监督管理局科技计划项目(2022008);中国药品监管科学行动计划第二批重点项目中药有效性安全性评价及全过程质量控制研究-中药材及饮片质量控制和评价方法研究(川牛膝);国家药监局2022年国家药品抽检中药饮片专项
中文摘要:目的:建立川牛膝中57种农药的液相色谱-质谱(LC-MS/MS)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(MRM)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,r2均大于0.993,57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。
中文关键词:川牛膝  农药残留  液相色谱-质谱法  生长调节剂  禁用农药  风险评估
 
Determination and risk assessment of 57 pesticide residues in Cyathulae Radix by LC-MS/MS
Abstract:Objective: To establish a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of 57 pesticides in Cyathulae Radix, and to use this method to detect pesticides in 348 batches of samples. Methods: The prepared samples were extracted with acetonitrile, then purified with QuEChERs package, determined by LC-MS/MS. Multiple reaction monitoring (MRM) was applied to collect data, and matrix matched standard curve method was selected for quantitation. The risk assessment and analysis of the detection results were carried out by the deterministic approach. Results: The calibration curves of all targets showed good linearity with correlation coefficients>0.993. The average recoveries for all target compounds ranged from 62.5% to 113.3%, with relative standard deviations<10.0%. 20 kinds of pesticides were detected in 348 batches of samples, including 4 kinds of banned pesticides, 6 plant growth regulators, 10 common pesticides. Risk assessment results show that the risk of pesticide residues in Cyathulae Radix was low, plant growth regulators were commonly used. Conclusion: The results show that the established method is sample, sensitive and accurate, and could be used for rapid screening and detection of multiple pesticide residues in Cyathulae Radix. The result has certain reference value for the pesticide risk assessment and standardized planting of Cyathula officinalis Kuan.
keywords:Cyathulae Radix  pesticide residue  LC-MS/MS  plant growth regulators  banned pesticides  risk assessment
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