摘要
选取桃仁、薏苡仁、肉豆蔻、地龙中药材为研究对象,进行黄曲霉毒素的测定方法学研究.采用高效液相色谱-柱后光化学衍生荧光检测法,分别从检测方法的专属性、检测限与定量限、线性与范围、重复性、中间精密度与溶液稳定性等6个方面进行检验分析和方法进行验证.结果表明:黄曲霉毒素G2、G1、B2、B1 分别在0.000 60～0.015 μg/kg、0.002 02～0.050 5 μg/kg、0.000 66～0.016 5 μg/kg、0.002 16～0.054 μg/kg范围内线性关系良好,R2=1.000(n=6);重复性试验黄曲霉毒素B1含量RSD为25.7％(n=6),含黄曲霉毒素G2、G1、B2、B1的总量RSD为24.4％(n=6);黄曲霉毒素对照品溶液在12 h内稳定性良好.桃仁、薏苡仁、肉豆蔻、地龙平均回收率分别为 84.6％、114.0％、84.3％、113.3％,RSD分别为 4.0％、4.8％、6.8％、5.7％(n=6).该检测方法专属性强、稳定性好、灵敏度高、结果准确可靠,为医药工作者在黄曲霉毒素检测和质量控制方面提供参考.
Abstract
The Chinese herbs including peach kernel,coix seed,nutmeg,and digolong were selected to establish the method for the determination of aflatoxins.The high performance liquid chromatography-post-column photo-chemically derived fluorescence detection method was used to test and analyze the specificity.This includes analyzing and validating the detection methods from six aspects:detection limit,quantitation limit,linearity,range,repeatability,intermediate precision and solution stability of the detection method.Through this process the method was further verified.The results show:Aflatoxins G2,G1,B2 and B1 had good linear relationships in the ranges of 0.000 60～0.015 μg/kg、0.002 02～0.050 5 μg/kg、0.000 66～0.016 5 µg/kg and 0.002 16～0.054 μg/kg,respectively.R2=1.000(n=6);The RSD of B1 content was 25.7% (n=6),and the total RSD of G2,G1,B2 and B1 was 24.4% (n=6).Aflatoxin control solution was stable within 12 hours.The average recoveries were 84.6% ,114.0% ,84.3% ,113.3% ,and the RSD were 4.0% ,4.8% ,6.8% ,5.7% (n=6),respectively.This detection method has strong specificity,good stability,high sensitivity,as well as accurate and reliable results,providing reference for pharmaceutical workers in the detection and quality control of aflatoxin.
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