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 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.