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超高效液相色谱-串联质谱法同时检测地龙药材中4种黄曲霉毒素含量及阳性结果确证 被引量:3

Simultaneous Determination of Four Aflatoxins in Pheretima by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry and Confirmation of Positive Results
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摘要 建立超高效液相色谱-串联质谱法同时测定地龙药材中黄曲霉毒素B1、B2、G1、G2的含量,并对阳性结果进行确证.样品经70%甲醇提取、免疫亲和柱净化、超高效液相色谱柱分离、三重四极杆质谱检测,并采用离子峰度比进行阳性结果确证.结果表明,4种黄曲霉毒素的线性关系良好(r>0.9995),回收率在91.2%~95.6%范围内.黄曲霉毒素B1、B2、G1、G2的检出限分别为0.10、0.038、0.11、0.038µg/kg.方法专属性好,灵敏度高,准确性好,可以进行最终阳性检出的判定.15批地龙药材中6批黄曲霉毒素确证阳性检出,证明地龙药材较易被黄曲霉毒素污染. A method for simultaneous determination of aflatoxins B1,B2,G1,and G2 in pheretima was been established by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS),and the positive results was confirmed.The samples were extracted by 70%methanol,purified by a immunoaffinity columns,separated by UPLC-MS/MS,detected by triple quadrupole mass spectrometry,and confirmed by ion peak ratio.The results showed that the linear relationship of the four aflatoxins were good(r>0.9995),and the recoveries ranged from 91.2%to 95.6%.The limits of detection for aflatoxin B1,B2,G1,and G2 were 0.10,0.038,0.11,0.038μg/kg,respectively.The method has a good specificity,high sensitivity,good accuracy,and can be used to determine the final positive detection.Aflatoxin were positively detected in 6 out of 15 batches of pheretima,which proved that the Pheretima were more susceptible to contamination by aflatoxins.
作者 郭晶 张进 李文君 李正刚 GUO Jing;ZHANG Jin;LI Wenjun;LI Zhenggang(Tonghua Institute for Food and Drug Control,Tonghua 134000,Jilin China;Siping Institute for Food and Drug Control,Siping 136000,Jilin China)
出处 《分析测试技术与仪器》 CAS 2024年第2期104-109,共6页 Analysis and Testing Technology and Instruments
基金 吉林省中药材标准及中药饮片炮制规范(项目编号:JLPZGF-2020-052)。
关键词 地龙 超高效液相色谱-串联质谱 黄曲霉毒素 阳性结果确证 Pheretima UPLC-MS/MS aflatoxin confirmation of positive results
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