建立了同时测定头发中10种蛋白同化激素液相色谱-串联质谱(LC/MS/MS)分析方法。头发样品经NaOH消解、戊烷液液提取后,用反相液相色谱分离,电喷雾正离子源进行离子化,用多反应监测方式(MRM)对这10种蛋白同化激素的母离子及子离子进行监测,三重四极杆质谱测定。10种蛋白同化激素的检出限为1~20ng/g;相对标准偏差(RSD)为1.72%~13.77%;回收率为38.20%~110.38%;线性回归系数(R^2)为0.9958~0.9999。本方法简便快速、灵敏度高、专属性强,可满足在兴奋剂检测或毒物分析中对毛发中蛋白同化激素测定的要求。
A sensitive and reproducible method for the quantitative detection of 10 kinds of anabolic androgenic steroids (AAS) has been developed. After decontamination steps, the hair sample (about 50 mg) was solubilised in 1 mL 1 mol/L NaOH, at 80℃ for 30 min, in the presence of 1 ng of epitestosterone-d3 used as internal standard. The homogenate was neutralized and extracted using a liquid-liquid extraction with pentane. The extract was separated by reversed phase liquid chromatography using methanol-water (containing 20 mmol/L ammonium acetate) as mobile phase. The AAS was confirmed and quantified using a API4000 MS-MS system in the multiple reaction monitoring mode via positive electrospray ionization. The calibration curves of the anabolic steroids were excellent with correlation coefficients (r) between 0.9958 and 0. 9998, RSD were between 1.7% and 13.8%, the recoveries were between 38. 2% and 110.4%, and the detection limits ranged from 1 to 20 ng/g. The established method is simple, rapid, sensitive and specific, and is appropriate for identification and quantification of anabolic steroids in human hair.