[关键词]
[摘要]
目的 采用免疫亲和净化HPLC柱后光化学衍生荧光检测法测定动物药中黄曲霉毒素,考察该方法在动物药黄曲霉毒素测定中的可行性。并对动物药中黄曲霉毒素污染情况进行筛查,为动物药的监管提供依据。方法 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。对部分动物药,尤其是可能污染黄曲霉毒素的动物药进行加样回收率考察,测定动物药中黄曲霉毒素残留量,并对测定结果进行分析。结果 动物药中黄曲霉毒素B1、B2、G1、G2的回收率均在70%~120%。16种64批动物药中有6种24批动物药检出了黄曲霉毒素,检出率为37.5%,其中4种13批动物药均出现了超过《中国药典》2015年版限度的现象,不合格率为20.3%。结论 免疫亲和净化HPLC柱后光衍生荧光检测法适用于动物药中黄曲霉毒素的测定。动物药的个别品种黄曲霉毒素污染情况较为严重,应尽快完善动物药的质量标准,保障用药安全。
[Key word]
[Abstract]
Objective To determine the aflatoxins residue of animal 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 in animal medicines was evaluated according to the determination data of aflatoxin contamination in animal medicines. Methods After extraction by organic solvent and purification by immunoaffinity column, aflatoxins samples were analyzed by HPLC with fluorescence detection after photochemistry derivation. The recovery rates of aflatoxins in animal medicines, especially the species easily contaminated by aflatoxin, were then determined by adding aflatoxin standard mixtures. Finally, aflatoxins in animal medicines were determined and the results were analyzed. Results Recovery rates of aflatoxin B1, B2, G1, and G2 were from 70% to 120%. Twenty-four batches of six kinds in 64 batches of 16 kinds of animal medicines were contaminated by aflatoxins, and the contamination rate was 37.5%. Thirteen batches of four kinds of animal medicines exceeded the limit of Chinese Pharmacopoeia of (2015 Edition), and the rate was 20.3%. Conclusion This method can be used to determine aflatoxins in animal medicines. Some species of animal medicines are likely to be contaminated by aflatoxins, so the aflatoxin control in those animal medicines should be put forward to ensure the safety of drug use.
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[基金项目]
国家十二五“重大新药创制”专项——中药质量安全检测和风险控制技术平台(2014ZX09304307-002)