自动固相萃取-HPLC-在线柱后光化学衍生法测定藿香正气水中黄曲霉毒素

Determination of Aflatoxin in Huoxiang Zhengqi Liquid by Automatic Solid Phase Extraction with HPLC and on Line Post Column Photochemical Derivatization

关键词:  黄曲霉毒素  藿香正气水  自动固相萃取  柱后光化学衍生  提取  净化

Key words:  aflatoxin  Huoxiang Zhengqi liquid  automatic solid phase extraction  post column photochemical derivation  extraction  purification

摘要:

目的 通过优化提取、净化和梯度洗脱程序建立藿香正气水中黄曲霉毒素（aflatoxin，AF）的测定方法。方法 采用免疫亲和柱自动固相萃取对样品提取液进行净化，通过HPLC-在线柱后光化学衍生荧光检测器检测，对全国18个生产企业的55批藿香正气水中AF进行检测。结果 AFB₁、AFB₂、AFG₁、AFG₂进样量分别在0.545~2.725，0.195~0.975，0.495~2.475，0.320~1.600 ng·mL^–1线性关系良好；平均加样回收率分别为94.90%，98.49%，94.17%，92.06%。在55批样品中均未检测出AF。结论 本法能有效去除杂质，排除色谱干扰，可作为藿香正气水中AF定量分析的检测方法。虽在55批样品中未检测出AF，但鉴于其处方饮片存在易被污染的风险，建议增加AF测定，以提高安全性。

Abstract:

OBJECTIVE To establish a method for the determination of aflatoxin in Huoxiang Zhengqi liquid through the optimization of extraction, purification and gradient elution prcedures.METHODS The sample extract was purified by automatic solid phase extraction with immunoaffinity column.And the AF was detected in 55 batches of Huoxiang Zhengqi liquid from 18 manufacturing enterprises nationwide by HPLC and on line post column photochemical derivatization fluorescence.RESULTS AFB₁, AFB₂, AFG₁ and AFG₂ had a good linear relationship within 0.545–2.725, 0.195–0.975, 0.495–2.475, 0.320–1.600 ng∙mL^–1 respectively.And the average recoveries of them were 94.90%, 98.49%, 94.17% and 92.06% respectively.AF was not detected in 55 batches of Huoxiang Zhengqi liquid.CONCLUSION The method can effectively remove impurities and eliminate chromatographic interference, and can be used for quantitative analysis of aflatoxin in Huoxiang Zhengqi liquid.Although AF is not detected in 55 batches of samples, it is suggested to increase the determination of AF in order to improve the safety in view of the risk of contamination of prescription pieces.