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超声提取-免疫亲和柱净化-柱后光化学衍生高效液相色谱法同时测定吉林省内蜂花粉中4种黄曲霉毒素

Simultaneous determination of four aflatoxins in Apis pollen in Jilin province by ultrasonic extraction-immunoaffinity column purification-post column photochemical derivatization HPLC
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摘要 本研究建立高效液相色谱法(HPLC)同时测定吉林省内蜂花粉药材中4种黄曲霉毒素含量的方法。将蜂花粉样品粉碎成细粉,用70%甲醇溶液超声处理35 min,续滤液经免疫亲和柱净化后,采用HPLC分离并结合光化学柱后衍生,通过荧光检测器测定AFB_(1)、AFB_(2)、AFG_(1)、AFG_(2)的含量。结果显示,4种黄曲霉毒素在一定质量范围内与相应的峰面积呈良好线性关系,r均大于0.9997;4种黄曲霉毒素的检出限分别为0.343、0.134、0.341、0.139μg/kg;样品平均回收率为92.3%~95.9%,RSD不大于2.6%(n=6)。该方法操作简单,灵敏度高且重复性好,可用于蜂花粉中黄曲霉毒素含量的测定。 A high performance liquid chromatography(HPLC)method was established for the simultaneous determination of four aflatoxins in Apis pollen medicinal materials in Jilin province.The samples were ultrasonically treated with 70%methanol solution for 35 minutes.The filtrate was purified by immunoaffinity column,separated by HPLC,and derivatized via a photochemical column derivation method.The contents of AFB_(1),AFB_(2),AFG_(1) and AFG_(2) were determined by fluorescence detector.The results showed that the four aflatoxins had a good linear relationship with the corresponding peak area in a certain mass range,and the r was greater than 0.9997.The detection limits of the four aflatoxins were 0.343,0.134,0.341 and 0.139μg/kg,respectively.The average recovery was 92.3%-95.9%,and RSD was no more than 2.6%(n=6).It can be seen that the method is simple,sensitive and reproducible,and can be used for the determination of aflatoxin content in Apis pollen.
作者 战宏利 刘东平 刘华 杨荣艳 马彧 ZHAN Hongli;LIU Dongping;LIU Hua;YANG Rongyan;MA Yu(Siping Institute for Food and Drug Control,Siping Jilin,136000,China;Jilin Jichun Pharmaceutical Limited Company)
出处 《质量安全与检验检测》 2025年第6期34-37,共4页 QUALITY SAFETY INSPECTION AND TESTING
基金 吉林省中药材地方标准制修订项目(JLZYC-2018-011)。
关键词 蜂花粉 黄曲霉毒素 高效液相色谱法 免疫亲和柱 光化学衍生 超声提取 Apis pollen Aflatoxin High perfoumance liquid chromatograph Immunoaffinity column Photochemical derivatization Ultrasonic extraction
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