免疫亲和柱净化-柱后光化学衍生-高效液相色谱荧光法测定保和系列制剂中黄曲霉毒素

Determination of aflatoxin G_2,G_1,B_2,B_1 in Baohe preparations by photochemical derivatization-HPLC-fluorescence detector

目的研究建立光化学柱后衍生-高效液相色谱(HPLC)-荧光检测器测定保和系列制剂中黄曲霉毒素G2、G1、B2、B1的方法。方法 70%甲醇提取样品,免疫亲和柱净化后,经高效液相色谱分离,由光化学柱后衍生,通过荧光检测器测定。结果在优化条件下,黄曲霉毒素G2、G1、B2、B1分别在0.064 6～3.230 ng、0.199 2～9.960 ng、0.068 4～3.420ng、0.195 4～9.770 ng的范围内有良好的线性关系,r>0.999 6,回收率在85.5%～114.6%之间,RSD>8。结论该方法快速简便,灵敏度高、重现性好,对68个生产企业生产的3个剂型148批保和制剂进行了检测,结果表明该方法可作为保和系列制剂中黄曲霉毒素的检测,保和制剂黄曲霉毒素状况较好。

AIM To study the method for determining aflatoxin G2,G1 ,B： ,B1 by photochemical derivatization- HPLC- fluorescence detector in Baohe preparations. METHODS The samples were extracted with 70% methanol and cleaned up with immuno affinity columns. The separation of aflatoxin G2, G1, B： and B1 was conducted by HPLC, the determination was carried outby fluorescence detector after photochemical derivatization. RESULTS Under optimum conditions, the calibration curves of aflatoxin G2, G1 , B2 and B1 were linear within the ranges of 0. 064 6 -3.230 ng, 0. 199 2 -9. 960 ng, 0. 068 4 -3. 420 ng and 0. 195 4 -9. 770 rig, respectively. The correlation coefficient was greater than 0. 999 6, and their recoveries were from 85.5% to 114. 6%. CONCLUSION The method is simple, sensitive and reproducible, which is suitable for the determination of aflatoxin in Baohe preparations.