中国药典黄曲霉毒素检测过程有关问题分析

Analysis about Determination of Aflatoxins in China Pharmacopoeia

目的探讨中药材黄曲霉毒素检验过程中的影响因素,比较现行方法与超高效液相色谱荧光检测器无衍生法。方法比较不同的碘浓度和流速对衍生效果的影响,不同的基质条件下不同品牌免疫亲和柱的回收率;用超高效液相色谱-荧光检测器无衍生快速测定柏子仁药材中4种黄曲霉毒素的含量。结果最终确定衍生方式为衍生溶液为0.01%碘溶液,衍生化泵流速0.4 m L/min;不同品牌的免疫亲和柱上的回收率差异较大;采用UPLC-FLR方法 AFB1与AFG1在0.2~20 ng/m L范围内、AFB2与AFG2在0.1~6.0 ng/m L范围内线性关系均良好,r〉0.999 9;4种黄曲霉毒素回收率在85.0%~99.0%之间。结论采用碘衍生测定黄曲霉毒素时可适当降低碘衍生溶液的浓度;采用UPLC-FLR方法检验黄曲霉毒素,方法快速、准确。

OBJECTIVE To discusse the influence factors in the determination process of the 4 aflatoxins（ B1,B2,G1,G2）.And to compare the current method with UPLC-FLR without derivatization. METHODS The effects of concentration of iodine solution and flow rates of derivative pump were studied,and the recovery rates of different brands of immune affinity column were compared in different matrix. The aflatoxins in Seman Platycladi were rapidly analyzed by UPLC-FLR without derivatization. RESULTS The I2 concentration was 0. 01%,with flow rate of 0. 4 m L / min. The recoveries had greater differences in several brands of immunoaffinity column. In UPLC-FLR,there was a good linearity over the ranges of 0.2-20 ng / m L for AFB1 and AFG1,0.1-6.0 ng/m L for AFB2 and AFG2,respectively. The average recoveries ranged from 85.0%-99.0%,r〉0.999 9. CONCLUSION It is suggested I2 concentration reduced with post-column derivatization. The UPLC-FLR method is quick and accurate.