Determination of cortisol in human saliva using liquid chromatography-electrospray tandem mass spectrometry
Determination of cortisol in human saliva using liquid chromatography-electrospray tandem mass spectrometry
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DOI：
10.1016/s1570-0232(02)00753-5
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发表时间：
2003-01-25
影响因子：
3
通讯作者：
Orbæk, P
中科院分区：
文献类型：
--
作者：
Jönsson, BAG;Malmberg, B;Orbæk, P
建立了唾液中皮质醇的液相色谱-串联质谱（LC-MS-MS）测定方法。在唾液管上对唾液取样。离心，加入氘标记的皮质醇作为内标，用乙腈沉淀蛋白质。将上清液蒸发，溶解在用乙酸酸化的甲醇中，并通过LC-MS-MS进行分析。通过合并志愿者的唾液样品，然后在单次运行中分析这些样品，检测运行内精密度，发现在0.7 μ l（-1）时为7%。通过在不同日期分析相同样品来测试运行间精密度，发现在2.5 μ g l（-1）时为11%。定量限为0.5 μ l（-1）。该方法被应用于分析的唾液样本从三名志愿者在他们的假期前的最后一周和第一和第二周的假期。此外，将该方法与免疫学方法分析进行了比较。免疫学方法的值是LC-MS-MS结果的2.7倍。(C)2002 Elsevier Science B. V.保留所有权利。
The aim of this work was to develop a method for determination of cortisol in saliva by liquid chromatography-tandem mass spectrometry (LC-MS-MS). Saliva was sampled on Salivette tubes. These were centrifuged, deuterium-labeled cortisol was added as internal standard and the proteins precipitated by acetonitrile. The supernatant was evaporated, dissolved in methanol acidified with acetic acid and analyzed by LC-MS-MS. The with-in run precision, tested by pooling saliva samples from volunteers and then analyzing these in a single run, was found to be 7% at 0.7 mug l(-1). The between-run precision was tested by analysis of the same samples at different days and found to be 11% at 2.5 mug l(-1). The limit of quantification was 0.5 mug l(-1). The method was applied for analysis of saliva samples from three volunteers during their last week before vacation and the first and second week on vacation. In addition, the method was compared to analysis by an immunological method. The values from the immunological method were 2.7 times higher than the LC-MS-MS results. (C) 2002 Elsevier Science B.V. All rights reserved.