免疫亲合柱净化HPLC柱后溴衍生化方法检测中药中黄曲霉毒素

目的采用免疫亲合柱净化,结合柱后衍生化的高效液相色谱荧光检测器检测常用中药材中的黄曲霉毒素B₁,B₂,G₁,G₂。方法样品经甲醇水(7∶3)溶液超声提取后,通过免疫亲合柱净化洗脱,再经过溴化溴化吡啶柱后衍生,高效液相色谱分离定量。结果B₂和G₂的最低检出限为006μg·kg^-1,B₁和G₁的最低检出限为020μg·kg^-1。回收率实验添加两个水平的标样,回收率904%～997%,RSD3%～12%。结论采用此方法检测常用中药材中的黄曲霉毒素无干扰性杂峰,结果准确可靠。

HPLC analysis of alfatoxins in medicinal herb extracts by immunoaffinity column cleanup and post-column bromination

OBJECTIVE: To develop a new and accurate method to quantify aflatoxins in medicinal herbs. METHOD: This method consists of sample extraction by using MeOH-H2O (7:3), followed by clean-up with an immunoaffinity column, and finally HPLC determination with fluorescence detection. Aflatoxins B1 and G1 are determined as their bromine derivatives, produced in an on-line post-column derivatization system. RESULT: The overall average recoveries for different medicinal herbs spiked at two levels of standards were from 90.4% to 99.7%. The detection limit was 0.06 microg x kg(-1) for aflatoxins G2 and B2, and 0.20 microg x kg(-1) for aflatoxins G1 and B1. CONCLUSION: The use of immunoaffinity column provides excellent cleanup of interfering substances. The method has been applied successfully to analyze 96 natural drugs.