桃仁、薏苡仁、肉豆蔻、地龙中黄曲霉毒素的测定方法学研究

Study on the Determination Methodology of Aflatoxin in the Chinese Herbs Peach Kernel,Coix Seed,Nutmeg,and Digolong

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0.00060~0.015μg/kg、0.00202~0.0505μg/kg、0.00066~0.0165μg/kg、0.00216~0.054μg/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。

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 photochemically 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 0.00060~0.015μg/kg、0.00202~0.0505μg/kg、0.00066~0.0165μg/kg and 0.00216~0.054μg/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.