液质联用法测定鲜蛋黄中的棉酚

采用HPLC-ESI-MS/MS联用技术,检测鲜蛋黄中的棉酚残留。样品经丙酮提取后,以C18柱为液相分离柱,以甲醇和1%甲酸为流动相,多反应监测模式测定棉酚,定性定量离子对分别为517.4/259.3、517.4/231.3。棉酚含量在1 ng/mL~100 ng/mL范围内具有良好的线性关系,测定下限(10 S/N)为1 ng/mL。以鲜蛋黄为基体,加入3种不同浓度水平的棉酚做加标回收试验,回收率在85%~100%之间,相对标准偏差(n=6)小于10%。该方法操作简单,结果准确,重现性好。

Determination of Gossypol in Egg Yolk by HPLC-MS

Determination of gossypol in egg yolk samples was studied by using HPLC-ESI-MS/MS.The sample was extracted with acetone and analyzed on a C18 column using methanol and 1% formic acid as mobile phase.The monitoring ions of gossypol were 517.4/259.3 and 517.4/231.3 in the multiple reaction monitoring mode(MRM).Linear relationship between values of peak area and mass concentration of gossypol was obtained in the range of 1 ng/mL~100 ng/mL,with lower limit detection(10 S/N) of 1 ng/mL.Recovery test was made by addition of standard gossypol with different concentrations.The recovery was found in the range of 85%-100%.RSD was found to be less than 10%(n=6).The method was simple,sensitive,accurate and repeatable.