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多预处理净化后采用高效液相色谱-荧光检测法测定 Ben Lamge 颗粒中的黄曲霉毒素 B1、B2、G1、G2

[Determination of aflatoxin B1, B2, G1, G2 in Ben Lamge granules by HPLC-FLD after multi-pretreatment clean-up].

作者信息

Zhang Qiong, Ran Cong-cong, Chen Dan, Li Jun-mei, Jiang Ye

出版信息

Zhongguo Zhong Yao Za Zhi. 2015 Oct;40(19):3780-5.

PMID:26975102
Abstract

To establish a multi-pretreatment method for the determination of aflatoxin B1, B2, G1, G2 in Chinese patent medicines, aflatoxins were analyzed by high performance liquid chromatography-fluorescence detector with post-column derivatization, after the multi-pretreatment of samples. The results showed that after the samples extracted with MeOH-H2O, dehydrated by anhydrous magnesium sulphate and sodium chloride, and finally purified by neutral alumina, the impurity interference of different sources in Chinese patent medicines matrix can be effectively removed, and the main peak can be nicely separated from the impurity peak. The detection limits were 0.25, 0.25, 0.50, 0.25 μg x L(-1) for AFB1, AFB2, AFG1, AFG2, respectively. The quantification limits were 1.00, 0.50, 1.00, 0.50 μg x L(-1), respectively. Aflatoxin B1, G1 showed a good linear relationship at a range of 1.0-50 μg x L(-1), aflatoxin B2, G2 at a range of 0.5-12.5 μg x L(-1) (R2 > 0.99). The average recovery was 80.40% - 108.6%. The present method is simple, reproducible with the reasonable recoveries and can be applied for the determination of aflatoxins in Chinese patent medicines.

摘要

为建立一种用于测定中成药中黄曲霉毒素B1、B2、G1、G2的多重预处理方法,在对样品进行多重预处理后,采用高效液相色谱-柱后衍生荧光检测器对黄曲霉毒素进行分析。结果表明,样品经甲醇-水提取、无水硫酸镁和氯化钠脱水、中性氧化铝最终净化后,可有效去除中成药基质中不同来源的杂质干扰,主峰与杂质峰能很好地分离。黄曲霉毒素B1、B2、G1、G2的检出限分别为0.25、0.25、0.50、0.25 μg·L⁻¹,定量限分别为1.00、0.50、1.00、0.50 μg·L⁻¹。黄曲霉毒素B1、G1在1.0 - 50 μg·L⁻¹范围内呈良好线性关系,黄曲霉毒素B2、G2在0.5 - 12.5 μg·L⁻¹范围内呈良好线性关系(R² > 0.99)。平均回收率为80.40% - 108.6%。本方法操作简便、重现性好、回收率合理,可用于中成药中黄曲霉毒素的测定。

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