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建立了食品中合成固醇类激素(群勃龙、勃地龙、诺龙、美雄酮、睾酮、司坦唑醇、甲基睾酮、黄体酮、丙酸诺龙、丙酸睾酮和苯丙酸诺龙)和糖皮质类激素(泼尼松龙、泼尼松、氢化可的松、地塞米松、倍他米松、甲基泼尼松、倍氯米松和氟氢可的松)多残留的液相色谱-串联质谱(LC-MS/MS)检测方法。样品经乙酸铵提取,甲醇再提取,加水混匀,ENVI-Carb固相柱和NH3固相柱净化,经C18柱分离后进行LC-MS/MS选择反应监测模式下定量分析。合成固醇类激素采用正离子模式检测,糖皮质激素采用负离子模式检测,一次前处理,2次进样。19种激素的定量检出限为0.1~1.0μg/kg;采用1,3和10倍定量进行分析,回收率在50%~110%之间,相对标准偏差为2.0%~12.0%。对134批次样品进行检测,统计得到内源性激素(黄体酮、氢化可的松和睾酮)的本底值。
Established in the food synthetic steroid hormones (trenbolone, vinpocetine, nandrolone, meloxone, testosterone, stanozolol, methyltestosterone, progesterone, nandrolone, testosterone propionate and benzene acid Nandrolone) and glucocorticoids (prednisolone, prednisone, hydrocortisone, dexamethasone, betamethasone, methylprednisone, beclometasone and fludrocortisone) Liquid chromatography - tandem mass spectrometry (LC-MS / MS) detection method. Samples were extracted with ammonium acetate, extracted with methanol, mixed with water, purified by ENVI-Carb solid phase column and NH3 solid phase column, and were separated by C18 column and quantified by LC-MS / MS selective reaction monitoring. Steroid hormone synthesis using positive ion mode detection, glucocorticoid negative ion mode detection, a pre-treatment, 2 injection. The detection limit of 19 hormones was 0.1 ~ 1.0μg / kg. The recoveries were between 50% and 110% with relative standard deviations of 2.0% ~ 12.0%. 134 batches of samples were tested and the background values of endogenous hormones (progesterone, hydrocortisone and testosterone) were obtained.