HPLC-光化学衍生法测定滋阴清热降糖丸中的黄曲霉毒素  

Determination of aflatoxin in Ziyin Qingre Jiangtang pills by HPLC-photochemical derivatization

作　　者：何元 顾崇梅 HE Yuan;GU Chongmei(Jiuquan Center of Drug Inspection and Testing in Gansu Province,Jiuquan Gansu 735000,China)

机构地区：[1]甘肃省酒泉市药品检验检测中心,甘肃酒泉735000

出　　处：《中兽医医药杂志》2022年第6期60-63,共4页Journal of Traditional Chinese Veterinary Medicine

基　　金：甘肃省药品监督管理局科研项目(2020GSMPA022)。

摘　　要：建立高效液相色谱-柱后光化学衍生法测定滋阴清热降糖丸中黄曲霉毒素AFG2、AFG1、AFB2、AFB1的含量。以Avantor Apollo C18(250.0 mm×4.6 mm, 5μm)为色谱柱,以甲醇-乙腈-水(45∶5∶50)为流动相,流速0.8 mL/min,柱温30℃,进样体积20μL。采用柱后光化学衍生-荧光检测器测定黄曲霉毒素,FLD激发波长360 nm,发射波长450 nm。结果显示,AFG2、AFG1、AFB2、AFB1进样量分别在0.76~30.40 pg、2.16~86.40 pg、0.76~30.40 pg、2.08~83.20 pg范围内与响应值线性关系良好,相关系数(r)均在0.995以上,加标回收率为80.6%~108.1%。该法可用于滋阴清热降糖丸中残留黄曲霉毒素的测定,方法快速准确、重复性好,可为滋阴清热降糖丸的安全性评价提供数据支持。A HPLC-post-column photochemical derivatization method was established to determine the contents of aflatoxin AFG2, AFG1, AFB2 and AFB1 in Ziyin Qingre Jiangtang pills. Avantor Apollo C18(250.0 mm×4.6 mm, 5 μm) was used as the chromatographic column, methanol-acetonitrile-water(45∶5∶50) was used as the mobile phase, flow rate was 0.8 mL·min-1, column temperature was 30℃, and the injection volume was 20 μL. Aflatoxin was determined by post-column photochemical derivatization-fluorescence detector. The excitation wavelength of FLD was 360 nm and the emission wavelength was 450 nm. A method for the determination of aflatoxin in Ziyin Qingre Jiangtang pills was established, and the linear relationship between the samples of AFG2, AFG1, AFB2 and AFB1 and the response values was good in the range of 0.76-30.40 pg, 2.16-86.40 pg, 0.76-30.40 pg and 2.08-83.20 pg, respectively, and the correlation coefficients(r) were all above 0.995, the recovery rate of standard addition was between 80.6% and 108.1%. This method can be used for the determination of aflatoxin residues in Ziyin Qingre Jiangtang pills, which is rapid, accurate and reproducible, and can provide data support for the safety evaluation of Ziyin Qingre Jiangtang pills.

关 键 词：HPLC-光化学衍射-FLD法 滋阴清热降糖丸 黄曲霉毒素 质量标准 

分 类 号：S853.7[农业科学—临床兽医学]