| 摘要: |
| 目的 建立一种方便、可靠和灵敏的液相色谱-串联质谱（LC-MS/MS）方法用于检测健康人唾液中2种内源性激素（睾酮和皮质醇）的水平。方法 在Agilent 6410A串联质谱仪上采用正离子检测模式，以卡马西平为内标，唾液样品经OMGEA NANOSEP 10K超滤管21 912.8×g超滤10 min后，在Agilent ZORBAX SB-C18（3.5 μm，2.1 mm×100 mm）色谱柱上采用等度洗脱进行色谱分离。流动相为乙腈：0.1%甲酸水溶液（60：40）；流速为0.3 mL/min；进样量为10 μL；柱温为25℃；每个样品的分析周期为3 min。结果 睾酮和皮质醇线性关系良好，其相关系数r>0.990，日内与日间精密度均<15%。结论 该方法可以用于测定唾液中睾酮和皮质醇的含量，为迅速简便地检测体内激素水平提供参考。 |
| 关键词: 液相色谱-串联质谱法 唾液 睾酮 皮质醇 内源性激素 |
| DOI：10.16781/j.0258-879x.2019.01.0104 |
| 投稿时间：2018-05-29修订日期：2018-11-15 |
| 基金项目:上海市临床药学重点专科建设项目（2016-40044-002），上海市卫生计生系统重要薄弱学科建设项目（2016ZB0303）. |
|
| Determination of testosterone and cortisol in saliva of healthy human by liquid chromatography-tandem mass spectrometry |
| GU Wei-feng1,LIANG Feng-ying2,LIU Lin-jing2,GAO Shou-hong2* |
(1. Department of Outpatient, Shanghai Naval Vessel Service Department, Shanghai 200083, China;
2. Department of Pharmacy, Changzheng Hospital, Naval Medical University(Second Military Medical University), Shanghai 200003, China
*Corresponding author) |
| Abstract: |
| Objective To establish a convenient,reliable and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of two kinds of endogenous hormones (testosterone,cortisol) in the saliva of healthy human.Methods A positive ion mode was performed on the Agilent 6410A mass spectrometer. Carbamazepine was used as the internal standard.The saliva samples were centrifuged at 21 912.8×g for 10 min with OMGEA NANOSEP 10K ultrafiltration tubes,and chromatographic separation was achieved on an Agilent ZORBAX SB-C18 column with isocratic elution.The mobile phase was acetonitrile:0.1% formic acid awter solution (60:40);flow rate was 0.3 mL/min;injection volume was 10 μL;column temperature was 25℃;and the analysis period of each sample was 3 min.Results Testosterone and cortisol had good linear relationship with correlation coefficient (r) being both >0.990.Inter-and intra-day precision was both less than 15%.Conclusion This method can be used to determine the contents of testosterone and cortisol in saliva,which provides a reference for rapid and simple detection of hormone levels in vivo. |
| Key words: liquid chromatography-tandem mass spectrometry saliva testosterone cortisol endogenous hormones |
