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目的建立液相色谱-串联质谱法快速检测鸡蛋中己烯雌酚的残留量。方法以乙腈为溶剂提取鸡蛋中的己烯雌酚,上清液用氮气吹干,加流动相溶解,正己烷脱脂后,液相色谱-电喷雾串联质谱负离子模式,选择反应监测(SRM)方式进行检测,定性离子对为m/z 267→m/z 251、m/z 267→m/z 237,其中m/z 267→m/z 251用于外标法定量。结果己烯雌酚的浓度为2.5 ng/ml~50 ng/ml时,线性关系良好,线性回归方程为y=4.32×104x-4.16×103,相关系数(r)为0.999 0。鸡蛋中己烯雌酚的定量检测限为0.5μg/kg(S/N=15)。在1.0μg/kg、5.0μg/kg、10.0μg/kg 3种加标水平下,己烯雌酚的平均回收率为88.0%~97.4%,相对标准偏差(RSD)为4.8%~8.7%。结论本法快速、灵敏、准确,可用于鸡蛋中己烯雌酚残留的痕量检测。
Objective To establish a liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for rapid determination of diethylstilbestrol in eggs. Methods The diethylstilbestrol was extracted from eggs with acetonitrile as solvent. The supernatant was dried under nitrogen, dissolved in mobile phase, defatted with hexane and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (Negative Ion Mode). The reaction was monitored by SRM. Qualitative ion pairs were m / z 267 → m / z 251, m / z 267 → m / z 237, where m / z 267 → m / z 251 was used for external standard quantification. Results When the concentration of diethylstilbestrol was 2.5 ng / ml ~ 50 ng / ml, the linear regression equation was y = 4.32 × 104x-4.16 × 103 and the correlation coefficient (r) was 0.999 0. The limit of detection of diethylstilbestrol in eggs was 0.5 μg / kg (S / N = 15). The average recoveries of diethylstilbestrol were 88.0% -97.4% with relative standard deviations (RSDs) of 4.8% -8.7% at the three spiked levels of 1.0μg / kg, 5.0μg / kg and 10.0μg / kg. Conclusion The method is rapid, sensitive and accurate and can be used for trace determination of diethylstilbestrol in eggs.