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固相净化结合超高效液相色谱-串联质谱法同时测定九香虫及其成方制剂中10种真菌毒素

Simultaneous Determination of 10 Mycotoxins in Aspongopus Chinensis and its Chinese Medicinal Preparations by UHPLC-MS after Solid Phase Purification
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摘要 目的:建立一种采用固相净化结合超高效液相色谱-串联质谱法(UHPLC-MS)同时测定九香虫及其3种成方制剂中10种真菌毒素的方法。方法:样品经乙腈-水-甲酸(84∶15.9∶0.1)提取,MFC100固相净化柱净化,采用UHPLC-MS在多反应监测(MRM)模式下进行测定,外标法定量。结果:10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>0.999),目标化合物在低、中、高3个质量浓度下的平均回收率为62.3%~106.6%(RSD<10%),定量限(LOQ)为0.17~88.04μg·kg^(-1)。结论:该法前处理步骤简便,净化效果良好,灵敏度高,准确性好,适合于九香虫及其成方制剂中10种真菌毒素的测定。 Objective:To develop a method for simultaneous determination of 10 mycotoxins in Aspongopus chinensis and 3 kinds of its Chinese Medicinal Preparations by UHPLC-MS/MS after solid phase purification.Methods:The samples were extracted with acetonitrile-water-formic acid(84∶15.9∶0.1)and purified by MFC100 solid phase purification columns.The mycotoxins were quantified by an external standard method.Results:The 10 mycotoxins showed good linearity within their respective concentration ranges(r>0.999).The average recoveries were 62.3%-106.6%(RSD<10%)at low,medium,and high spiked levels.The LOQs were in the range of 0.17-88.04μg·kg^(-1).Conclusion:The method based on simple pretreatment steps is accurate,sensitive and suitable for the simultaneous determination of 10 mycotoxins in Aspongopus chinensis and its Chinese medicinal preparations.
作者 胡珀 卜媛媛 赵祥杰 何晓希 金鹏 HU Po;BU Yuanyuan;ZHAO Xiangjie;HE Xiaoxi;JIN Peng(Huai'an Institute for Food and Drug Control,Huai'an 223001,China;Huaiyin Institute of Technology,Huai'an 223001,China)
出处 《药学与临床研究》 2023年第4期309-312,共4页 Pharmaceutical and Clinical Research
基金 江苏省市场监督管理局科技计划项目(KJ2022048)。
关键词 MFC100固相净化柱 九香虫 真菌毒素 超高效液相色谱-串联质谱法 MFC100 Solid phase purification column Aspongopus chinensis Mycotoxins UHPLC-MS/MS
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