舒肝丸中的黄曲霉毒素B_1、B_2、G_1、G_2的含量测定及安全性评价

Content Determination and Safety Evaluation of Aflatoxins B_1,B_2,G_1 and G_2 in Shugan Pills

目的:采用高效液相色谱法(HPLC)测定舒肝丸中黄曲霉毒素B_1、B_2、G_1、G_2的含量,并评价舒肝丸中黄曲霉毒素安全性。方法:采用C_(18)柱,流动相为甲醇-乙腈-水(10∶30∶60),色谱柱资生堂C_(18)(150 mm×4.6 mm,5μm),紫外光灯(254nm)衍生,荧光检测器,激发波长λex=360 nm,发射波长λem=450 nm,并对全国流通领域的舒肝丸中黄曲霉毒素B_1、B_2、G_1、G_2进行测定。结果:建立的HPLC法,黄曲霉毒素B_1、G_1在10~50 pg,黄曲霉毒素B_2、G_2在3~15 pg范围内线性良好;平均回收率分别为89.9%,87.9%,86.1%,87.1%,RSD均在3.0%以内。且经对全国流通领域的舒肝丸进行测定,结果全部样品的黄曲霉毒素B_1、B_2、G_1、G_2含量均符合要求,合格率为100%,表明安全性较好。结论:该分析方法操作简便、快速、结果稳定、准确,可为舒肝丸的定量分析方法及安全性评价。

Objective：To determine aflatoxin B1 , B2 , G1 and G2 in Shugan pills by HPLC and evaluate their safety. Methods：The product was analyzed by HPLC using a Shiseido C18 column（150 mm ＆#215; 4. 6 mm,5 μm）with methanol-acetonitrile-water （10 ：30 ：60） as the mobile phase. An ultraviolet lamp was derivative at 254 nm, and the fluorescence detection was performed with the excitation wavelength at 360 nm and the emission wavelength at 450nm. The samples from nation-wide market were detected by the method. Re-sults：Good linear relationships were obtained within the range of 10-50 pg for aflatoxin B1 and G1 , and 3-15 pg for aflatoxin B2 and G2 . The recovery of aflatoxin B1 , B2 , G1 and G2 was 89. 9%,87. 9%,86. 1% and 87. 1%,respectively with all the RSD below 3. 0%. The results of all samples were satisfactory, and the qualification rate of the samples was 100%, indicating that the samples were safe. Conclusion：The developed method is convenient and accurate, which can be applied in the quantitative determination of Shugan pills.