高效液相色谱-串联质谱法同时检测鸡肉和鸡蛋中合成类固醇类激素和糖皮质激素

Determination of Anabolic Steroid and Glucocorticoid Hormones in Chicken and Egg Using Liquid Chromatography-Tandem Mass Spectrometry

建立了鸡肉和鸡蛋中合成类固醇类激素(睾酮、甲基睾酮、群勃龙、勃地龙、诺龙、美雄酮、司坦唑醇、丙酸诺龙、丙酸睾酮及苯丙酸诺龙)和糖皮质类激素(泼尼松、泼尼松龙、地塞米松、氟氢可的松、甲基泼尼松、倍氯米松及氢化可的松)多残留的液相色谱-串联质谱(LC-MS/MS)检测方法。样品经乙腈超声提取,正己烷脱脂净化,以甲醇-甲酸水溶液为流动相,经C18柱分离后进行LC-MS/MS选择反应监测模式下的定性及定量分析。合成类固醇类激素采用正离子模式检测,糖皮质激素则采用负离子模式检测,正、负离子化模式一次进样同时检测。类固醇类和糖皮质类激素的定量检出限为0.5μg/kg。在0.5、1.0和5.0μg/kg3种浓度添加水平,上述激素的平均回收率为73.4%～108.9%;相对标准偏差为3.4%～13.4%。可实现样本灵敏、准确地定性定量分析。

A liquid chromatography-tandem mass spectrometric （LC-MS/MS） method was developed for the simultaneous identification and determination of multi-residues amounts of anabolic steroid hormones testosterone, methyl testosterone, trenbolone, boldenone, nandrolone, methandienone, stanozolol, nandrolone, propi- onate testosterone, propionate nandrolone, phenylpropionate, and glucocorticoids prednisone, prednisolone, hydrocortisone, methylprednisolone, dexamethasone, beclomethasone, fludrocortisone in chicken and egg.Homogenized tissue samples were extracted with acetonitrile under ultrasonication incubation. Clean-up proce- dure was carried out with hexane liquid-liquid partition. After Cls LC gradient elution separation using metha- nol and formic solution as mobile phase, the eluents were qualitatively and quantitatively determined under selected-reaction monitoring （SliM） scan type with tandem mass analyzer using positive polarity mode for the anabolie steroid hormones and negative polarity for the glueoeortieoid hormones. All the positive and negative ions were detected in one injection at the same time. The limit of quantitation （LOQ） for the above hormones was 0.5 μg/kg. At three spiked levels, 0.5, 1.0 and 5.0μg/L, the mean recoveries were within the range from 73.4% to 108.9% , and the relative standard deviation was in the range of 3.4% - 13.4%. The real sample test showed that this method could be used for sensitive~ and accurate determination of multi-class hormones residues in chicken and egg samples.