摘要
目的:通过优化黄曲霉毒素提取与净化方法来建立延胡索中黄曲霉毒素的测定方法。方法:采用免疫亲和柱净化-HPLC法测定,样品经超声提取后通过免疫亲合柱,用1%吐温-20的PBS溶液去除杂质,采用柱后光化学衍生荧光检测器检测,并对超出现行药典规定限度的样品用高效液相色谱-串联质谱(HPLC-MS/MS)法验证。结果:23批样品中有10批检出黄曲霉毒素,其中4批超出药典规定限度,超限样品与HPLC-MS/MS验证结果一致。结论:该方法能有效去除样品中的杂质,排除测定干扰,可作为延胡索中黄曲霉毒素定量分析的检测方法。10批样品均检出黄曲霉毒素,显现出黄曲霉毒素污染方面的安全问题,建议增加延胡索中黄曲霉毒素检查项,以确保药材质量的安全性、有效性。
Objective: To establish a method for determining aflatoxin in Rhizoma Corydalis by optimizing the extraction and purification method for aflatoxin. Methods: The sample was subjected to immunoaffinity column purification-HPLC. The sample was ultrasonically extracted and passed through an immunoaffinity column. The impurities were removed with 1% Tween-20 in PBS and the samples were detected by a post-column optical chemical derivatization fluorescence detector. The samples beyond the limits of the current pharmacopoeia were validated by HPLC/MS/MS mass spectrometry. Results: Aflatoxin was detected out from 10 batches of the 23 samples,and among them,4 ones exceeded the limits set by the pharmacopoeia,which were consistent with the mass spectrometry results. Conclusion: The method can effectively remove impurities in the samples and eliminate measurement interference,which can be used as a detection method for the quantitative analysis of aflatoxin in Rhizoma Corydalis. Aflatoxins were detected out from 10 batches of samples,highlighting the safety of aflatoxin contamination. It is recommended to strengthen aflatoxin test for Rhizoma Corydalis to ensure the safety and efficacy of the drug.
作者
张伟
谌宇
施思
伍勋
卢智玲
Zhang Wei;Shen Yu;Shi Si;Wu Xun;Lu Zhiling(Hangzhou Institute for Food and Drug Control,Hangzhou 310017,China)
出处
《中国药师》
CAS
2019年第10期1810-1814,共5页
China Pharmacist
基金
杭州市农业与社会发展科研自主申报项目(编号:2019203B71)
关键词
黄曲霉毒素
提取与净化技术
延胡索
Aflatoxin
Extraction and purification technology
Rhizoma Corydalis
