HPLC法测定土鳖虫中黄曲霉素的含量

摘要

OBJECTIVE:To establish a method for content determination of aflatoxins in eupolyphaga. METHODS:HPLC was performed on the column of Phenomenex-C18 with mobile phase of methanol-acetonitrile-water(28∶17∶55,V/V/V)at flow rate of 1.0 ml/min,column temperature was 30 ℃,fluorescence detector(FLD)λex was 365 nm,λem was 450 nm;derivative solution was 0.05% iodine solution,derivatized pump flow rate was 0.3 ml/min,derivatized temperature was 70 ℃ and volume injection was 20μl. RESULTS:Aflatoxin G2 and aflatoxin B2 showed good linear relationship at 1.2-12 pg,and aflatoxin G1 and aflatoxin B1 showed a good linear relationship at 4-40 pg(r≥0.999 3);RSDs of precision,stability and reproducibility tests were≤2.3%;aver-age recovery was 77.4%-94.8%(RSD=3.1%-4.3%,n=6). CONCLUSIONS:The method is simple,accurate and reproducible, and can be used for the determination of aflatoxins in eupolyphaga.%目的：建立测定土鳖虫中黄曲霉素含量的方法。方法：采用高效液相色谱法。色谱柱为Phenomenex C18，流动相为甲醇-乙腈-水（28∶17∶55，V/V/V），流速为1.0 ml/min，柱温为30℃，荧光检测器激发波长λex为365 nm，发射波长λem为450 nm，衍生溶液为0.05％碘溶液，衍生化泵流速为0.3 ml/min，衍生化温度为70℃，进样量为20μl。结果：黄曲霉素G2、黄曲霉素B2的进样量在1.2～12 pg，黄曲霉素G1、黄曲霉素B1进样量在4～40 pg范围内与各自峰面积呈良好线性关系（r均≥0.9993）；精密度、稳定性、重复性试验的RSD≤2.3％；加样回收率为77.4％～94.8％，RSD为3.1％～4.3％（n＝6）。结论：本方法简便、准确、重复性好，可用于测定土鳖虫中黄曲霉素的含量。