国际标准在川芎农药残留检测中的应用

Application of international standards in the determination of pesticide residues in Szechwan Lovage Rhizome

董自艳 ¹马晓英 ¹宋玉华 ²章晨峰 ¹王团结 ¹刘茫茫¹

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作者信息

1. 中药制药过程控制与智能制造技术全国重点实验室,江苏康缘药业股份有限公司,江苏连云港 222001
2. 梅里埃检测技术(青岛)有限公司,山东青岛 266000
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摘要

按照FDA和欧盟法规的农药种类、限度以及方法验证要求,采用改良的QuEChERS法结合液相色谱-串联质谱技术,建立川芎中54种农药残留检测方法.样品使用1％乙酸水溶液充分浸泡,经乙腈提取,Cleanert MSA-Q盐包盐析分层,QuEChERS净化,液相色谱-串联质谱检测,并采用过程校正标准曲线法进行定量.结果表明,54种农药线性关系良好,决定系数(R2)均大于0.99;在0.01、0.05和0.1 mg/kg加标水平下,加标回收率为92.5％～105.5％,日内精密度为0.4％～6.6％,日间精密度为1.0％～11.7％.方法操作简单、快速、准确,适用于川芎中多农药残留的高通量检测.

Abstract

According to FDA and EU regulations on pesticides,residue limits,and method validation requirements,a detection method for 54 pesticide residues in Szechwan Lovage Rhizome was established using a modified QuEChERS method combined with LC-MS/MS.The samples were soaked with acetic acid aqueous solution 1％,extracted by acetonitrile,purified by QuEChERS,detected by LC-MS/MS,and procedural standard calibration method was used for quantification.The results showed that the linear relationships of 54 pesticides were good,and the correlation coefficients(R2)were over 0.99.At the three spiked levels of 0.01,0.05 and 0.1 mg/kg,the average recoveries were 92.5％-105.5％,intra-day RSD(n=5)were 0.4％-6.6％and inter-day RSD(n=10)were 1.0％-1 1.7％.The method was simple,fast,accurate,and suitable for high-throughput detection of pesticide residues in Szechwan Lovage Rhizome.

关键词

国际法规/QuEChERS/液相色谱-串联质谱/川芎/农药残留/检测

Key words

international standard/QuEChERS/LC-MS/MS/Szechwan Lovage Rhizome/pesticide residue/determination

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基金项目

国家重点研发计划(2021YFC1712802)

出版年

2024

现代农药

江苏省农药协会江苏省农药研究所股份有限公司江苏省农药科技信息站

现代农药

CSTPCD

影响因子：0.471

ISSN：1671-5284

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