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

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(R^(2))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。

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(R^(2))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%-11.7%.The method was simple,fast,accurate,and suitable for high-throughput detection of pesticide residues in Szechwan Lovage Rhizome.