液相色谱-串联质谱法检测血清中15种甾体激素的动态变化

发布时间：2018-09-17 16:48

【摘要】：建立了用液相色谱-串联质谱检测血清中15种甾体激素的方法。在血清样品中加入含内标的乙腈沉淀蛋白质后,用100 mmol/L盐酸羟胺衍生,经Agilent-C18柱(50 mm×3.0 mm,2.7μm)分离,内标法定量。质谱分析采用电喷雾电离(ESI)正离子扫描,多反应监测(MRM)模式检测。数据显示,13种激素在0.05~20 ng/mL范围内线性关系良好(相关系数(R2)不小于0.995 6),检出限不大于1 ng/mL;皮质醇及脱氢表雄酮硫酸酯在50~2 000ng/mL范围内线性关系良好(R2不小于0.997 9),检出限不大于0.5 ng/mL。将该方法应用于女性月经周期激素变化规律的研究,结果表明,15种甾体激素在一个完整的月经周期内有不同特征的动态变化,其中雄激素在滤泡期的后期达到最高值,孕(雌)激素在黄体期达到最高值,而皮质激素则波动不明显。该方法灵敏度高、重复性好,为临床诊疗提供了参考。
[Abstract]:A method for the determination of 15 steroid hormones in serum by liquid chromatography-tandem mass spectrometry (LC-MS) was established. The protein containing internal standard acetonitrile was added to the serum sample. The protein was derived by 100 mmol/L hydroxylamine hydrochloride and separated by Agilent-C18 column (50 mm 脳 3.0 mm,2.7 渭 m). Electrospray ionization (ESI) positive ion scanning and multi-reaction monitoring (MRM) mode were used for mass spectrometry analysis. The data showed that there was a good linear relationship between the 13 hormones in the range of 0.05 ~ 20 ng/mL (R ~ 2 > 0.995 6), the detection limit was not more than 1 ng/mL; cortisol and dehydroepiandrosterone sulfate in the range of 50 000ng/mL (R2 > 0.997 9), and the detection limit was not more than 0.5 ng/mL.. The results showed that 15 steroid hormones had different dynamic changes in a complete menstrual cycle, androgen reached the highest value in the later stage of follicular period. The pregnant (estrogen) hormone reached the highest value in the luteal phase, while the corticosteroid did not fluctuate significantly. The method is sensitive and reproducible, and provides a reference for clinical diagnosis and treatment.
【作者单位】：浙江中医药大学;绍兴第二医院检验科;
【基金】：浙江省医药卫生科技计划项目(2014KYB285) 浙江省中医药科技计划(2012ZA066)~~
【分类号】：O657.63;R446.1

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