摘要
目的:建立QuEChERS结合超高效液相色谱-串联质谱法(UHPLC-MS)同时测定6种含土鳖虫的成方制剂中9种真菌毒素的方法。方法:样品用QuEChERS方法进行前处理,经10%甲酸乙腈提取,用N-丙基-乙二胺硅烷和无水硫酸镁进行净化,采用UHPLC-MS在多反应监测模式下进行测定,外标法定量。结果:9种真菌毒素的含量在各自质量浓度范围内具有较好的线性关系(r≥0.9956),目标化合物在低、中、高3个质量浓度下的平均回收率为70.42%~101.28%,RSD<12%,定量限(LOQ)为1.2~18.6μg·kg^(–1)。结论:该方法灵敏度高、准确性好,适合于土鳖虫及其成方制剂中9种真菌毒素的测定。
Objective:To develop a method for simultaneous determination of 9 mycotoxins in Eupolyphaga Steleophaga and 6 kinds of Chinese medicinal preparations containing Eupolyphaga Steleophaga by ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS)combined with QuEChERS.Methods:The samples were pretreated with QuEChERS,extracted with 10%formic acid in acetonitrile,purified by primary-secondary amine(PSA)and anhydrous magnesium sulfate.UHPLC-MS was employed for the quantification and confirmation of 9 mycotoxins with the external standard method.Results:The 9 mycotoxins showed good linearity within their respective concentration range(r≥0.9956).The average recoveries were 70.42%-101.28%(RSD<12%)under low,medium,and high spiked levels.The LOQs were in the range of 1.2-18.6μg·kg^(-1).Conclusion:This method is accurate,sensitive,and suitable for the determination of 9 mycotoxins in Eupolyphaga Steleophaga and Chinese medicinal preparations containing Eupolyphaga Steleophaga.
作者
李媛
张楠
张亚锋
孙晓
张苗苗
谢志民
LI Yuan;ZHANG Nan;ZHANG Ya-feng;SUN Xiao;ZHANG Miao-miao;XIE Zhi-min(Xi'an Institute for Food and Drug Control,Xi'an 710054,China)
出处
《中国现代中药》
CAS
2022年第1期142-146,共5页
Modern Chinese Medicine
基金
食品安全风险物质筛查检测服务平台建设项目(2019PT-22)。
