| 刘晶晶,李耀磊,王晶娟,戴忠,马双成.HPLC柱后光化学衍生荧光检测法检测3种含土鳖虫中成药的黄曲霉毒素[J].中国药事,2021,35(3):307-314 |
| HPLC柱后光化学衍生荧光检测法检测3种含土鳖虫中成药的黄曲霉毒素 |
| Determination of Aflatoxins in Three Chinese Patent Medicines Containing Euplyphaga Steleophaga by Immunoaffinity Column and High Performance Liquid Chromatography Coupled with Post-column Photochemical Derivatization |
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| DOI：10.16153/j.1002-7777.2021.03.010 |
| 中文关键词: 中成药 免疫亲和柱 黄曲霉毒素 B1 黄曲霉毒素 B2 黄曲霉毒素 G1 黄曲霉毒素 G2 风险评估 |
| 英文关键词: Chinese patent medicines immunoaffinity column aflatoxin B1 aflatoxin B2 aflatoxin G1 aflatoxin G2 risk assessmen |
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| 中文摘要: |
| 目的：考察免疫亲和净化HPLC柱后光化学衍生荧光检测法在中成药中黄曲霉毒素测定的可行性，并对其污染情况进行筛查，为中成药黄曲霉毒素污染监管提供依据。方法：采用免疫亲和净化 HPLC柱后光化学衍生荧光检测法对含有土鳖虫的中成药中黄曲霉毒素的含量进行测定。样品经有机溶剂提取、免疫亲和柱净化后，利用高效液相色谱-光化学衍生-荧光检测器进行分析测定。对3种含土鳖虫的中成药，考察加样回收率，测定黄曲霉毒素残留量，并对测定结果进行分析。采用高效液相色谱- 串联质谱法对部分超出限度批次进行结果确认。结果：3种中成药中黄曲霉毒素B1、B2、G1、G2的回收率均在80%~113%。3种24批中成药中，21批检出黄曲霉毒素，检出率为87.5%，部分批次黄曲霉毒素含量明显偏高。结论：免疫亲和净化HPLC柱后光衍生荧光检测法结果准确，重现性好，可用于中成药中黄曲霉毒素的测定。含土鳖虫药材的中成药，个别品种黄曲霉毒素污染情况较为严重，存在安全隐患，应引起生产企业的重视，保障用药安全。 |
| 英文摘要: |
| Objective: To determine the aflatoxins residue of Chinese patent medicines by immunoaffinity column HPLC method with post column photochemical derivatization and fluorescence detection, and to evaluate the feasibility of this method. The contamination status of aflatoxins was screened to provide basic data for the supervision of aflatoxin pollution. Methods: The aflatoxins residue of Chinese patent medicines containing Euplyphaga Steleophaga was determined by immunoaffinity column HPLC method with post column photochemical derivatization and fluorescence detection. After extraction by organic solvent andpurification by immunoaffinity column, aflatoxins samples were analyzed by HPLC with fluorescence detection after photochemistry derivation. The sample recovery rates of aflatoxins residue in 3 kinds of Chinese patent medicines containing Euplyphaga Steleophaga were determined by adding aflatoxin standard mixtures, and the results were analyzed. High performance liquid chromatography tandem mass spectrometry was used to confirm the results of some of the batches exceeding the limits. Results: Recovery rates of aflatoxin B1, B2, G1, and G2 were between 80% and 113% in 3 kinds of Chinese patent medicines. 21 out of 24 batches of 3 kinds of Chinese patent medicines were contaminated by aflatoxins, and the contamination rate was 87.5%. The content of aflatoxin in some batches was significantly high. Conclusion: The immunoaffinity column HPLC method with post column photochemical derivatization and fluorescence detection assay is accurate, reproducible and could be used to determine aflatoxins in Chinese patent medicines. The aflatoxin contamination of individual species of Chinese patent medicines containing Euplyphaga Steleophaga is serious, and there are potential safety hazards, which should be paid attention to by manufacturers to ensure the safety of medication. |
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