【摘要】：建立了用液相色譜-串聯(lián)質(zhì)譜檢測血清中15種甾體激素的方法。在血清樣品中加入含內(nèi)標(biāo)的乙腈沉淀蛋白質(zhì)后,用100 mmol/L鹽酸羥胺衍生,經(jīng)Agilent-C18柱(50 mm×3.0 mm,2.7μm)分離,內(nèi)標(biāo)法定量。質(zhì)譜分析采用電噴霧電離(ESI)正離子掃描,多反應(yīng)監(jiān)測(MRM)模式檢測。數(shù)據(jù)顯示,13種激素在0.05~20 ng/mL范圍內(nèi)線性關(guān)系良好(相關(guān)系數(shù)(R2)不小于0.995 6),檢出限不大于1 ng/mL;皮質(zhì)醇及脫氫表雄酮硫酸酯在50~2 000ng/mL范圍內(nèi)線性關(guān)系良好(R2不小于0.997 9),檢出限不大于0.5 ng/mL。將該方法應(yīng)用于女性月經(jīng)周期激素變化規(guī)律的研究,結(jié)果表明,15種甾體激素在一個完整的月經(jīng)周期內(nèi)有不同特征的動態(tài)變化,其中雄激素在濾泡期的后期達到最高值,孕(雌)激素在黃體期達到最高值,而皮質(zhì)激素則波動不明顯。該方法靈敏度高、重復(fù)性好,為臨床診療提供了參考。
[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.
【作者單位】： 浙江中醫(yī)藥大學(xué);紹興第二醫(yī)院檢驗科;
【基金】：浙江省醫(yī)藥衛(wèi)生科技計劃項目(2014KYB285) 浙江省中醫(yī)藥科技計劃(2012ZA066)~~
【分類號】：O657.63;R446.1

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