GC-MS/MS法检测肠炎宁片及其药材中禁用农药残留

Determination of Banned Pesticide Residues in Changyanning Tablets and Its Medicinal Materials by GC-MS/MS Method

目的建立同时定量分析肠炎宁片及其原料药材地锦草、金毛耳草中31个禁用农药残留的方法。方法用乙腈提取样品,再经改良后的Quick(快速)-Easy(容易)-Cheap(便宜)-Effective(有效)-Rugged(稳定)and Safe(可靠)(QuEChERS)方法进行净化,使用气相色谱-三重四极杆质谱仪(GC-MS/MS)检测,样品分析采用基质匹配标准曲线定量法。结果所建立的方法学考察均合格,平均回收率为72.0%~113.0%,相对标准偏差(RSD)为2.4%~17.8%。经过检测,并未检出《中国药典》2020年版通则0212项下规定的禁用农药。结论该方法精密度和重复性良好,能够快速、简便地完成禁用农药检测,可用于肠炎宁片的安全性监测。

Objective To develop a technique for the quantitative and simultaneous analysis of 31 pesticide residues that are prohibited in changyanning tablets and its raw ingredients.Methods The samples were extracted using acetonitrile,purified using a modified quick-easy-cheap-effective-rugged and safe(QuEChERS)procedure,and identified using GC-MS/MS.The samples were analyzed by matrix matching standard curve quantitative method.Results All the established methods were qualified,with average recoveries of 72.0%-113.0%and RSD of 2.4%-17.8%.The actual sample test results showed that all prohibited pesticides were not detected,in line with the provisions of General Rule 0212 of Chinese Pharmacopoeia 2020 edition.Conclusion The method is rapid,simple,accurate and repeatable,and can be used for the safety monitoring of changyanning tablets.