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建立了一种复合前处理手段应用于中成药中的黄曲霉毒素B1,B2,G1,G2的HPLC测定方法。样品经复合前处理方法处理后,用高效液相色谱-柱后衍生-荧光检测技术测定痕量黄曲霉毒素。结果表明,样品经甲醇-水系统提取、无水硫酸镁和氯化钠脱去水分、中性氧化铝吸附后,能有效去除中成药基质中不同基源的杂质干扰,待测峰和杂质峰分离度良好。4种目标分析物(AFB1,AFB2,AFG1,AFG2)的检出限分别为0.25,0.25,0.50,0.25μg·L-1,定量限分别为1.00,0.50,1.00,0.50μg·L-1,AFB1,AFG1线性范围1.0~50μg·L-1,AFB2,AFG2线性范围0.5~12.5μg·L-1,R2>0.99。平均回收率为80.40%~108.6%。该方法操作简单、重复性好、回收率较高,适用于中成药中黄曲霉毒素的快速分析。
An HPLC method for the determination of aflatoxins B1, B2, G1 and G2 in Chinese patent medicines was established by using a combination of pre-treatment methods. After the sample was treated by compound pretreatment, trace aflatoxin was determined by high performance liquid chromatography - post column derivatization - fluorescence detection. The results showed that the sample was extracted by methanol-water system, dehydrated by anhydrous magnesium sulfate and sodium chloride, and adsorbed by neutral alumina could effectively remove impurity interferences from different base sources in traditional Chinese medicine (TCM) matrix. Peaks and impurity peaks Good separation. The detection limits of the four target analytes (AFB1, AFB2, AFG1 and AFG2) were 0.25,0.25,0.50,0.25μg · L-1, and the limits of quantitation were 1.00,0.50,1.00,0.50μg · L-1, AFB1, AFG1 linear range of 1.0 ~ 50μg · L-1, AFB2, AFG2 linear range of 0.5 ~ 12.5μg · L-1, R2> 0.99. The average recovery was 80.40% ~ 108.6%. The method has the advantages of simple operation, good repeatability and high recovery rate, and is suitable for rapid analysis of aflatoxins in proprietary Chinese medicines.