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[液相色谱串联质谱法测定唾液中的皮质醇]

[Determination of Cortisol in Saliva by Liquid Chromatography Tandem Mass Spectrometry].

作者信息

Liu X D, Qiao H, Meng X J, Wang C, Ding X W, Niu D S, Li J

机构信息

The Beijing Prevention and Treatment of Hospital of Occupational Disease for Chemical Industry, Beijing 100093, China.

The Beijing Prevention and Treatment of Hospital of Occupational Disease for Chemical Industry, Beijing 100093, China; Beijing University of Chemical Technology, Beiijng100029, China.

出版信息

Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi. 2019 Feb 20;37(2):143-146. doi: 10.3760/cma.j.issn.1001-9391.2019.02.014.

Abstract

To establish a liquid chromatography tandem mass spectrometry method to determine the cortisol in saliva. Take 0.5 ml saliva sample into a 2 ml centrifuge tube, add excess sodium chloride and 1ml acetonitrile to it, then vortex for 3 min, centrifuge for 10 min at 15 000 r/min, and take 800 μl of the upper layer to another centrifuge tube. Finally, the sample was concentrated by a vacuum concentrator and brought to 200 μl with the initial mobile phase. Then, the sample was analyzed by liquid chromatography tandem mass spectrometry. The target compound was quantified by external standard curve method. The linear range of the method was 0.025.00 ng/ml, =0.999 9, the method limit of the detection was 0.002 ng/ml, the method limit of quantitative was 0.02 ng/ml, and the spiked recoveries were 89.60%98.60%. The intraassay precision was 1.90%3.30%, and the interassay precision was 4.20%9.00%; samples could be stored at -20 °C for at least 14 days. The determination of cortisol could not be interfered by other endogenous substances in the sample. The method is simple in pretreatment, high sensitivity, good reproducibility and good recovery, and it is suitable for the quantitative analysis of cortisol in saliva for normal and occupationally stressed populations.

摘要

建立液相色谱串联质谱法测定唾液中皮质醇的含量。取0.5 ml唾液样本置于2 ml离心管中,加入过量氯化钠和1 ml乙腈,涡旋3 min,于15 000 r/min离心10 min,取上层800 μl转移至另一离心管。最后,样本经真空浓缩仪浓缩,并用初始流动相定容至200 μl。然后,采用液相色谱串联质谱法对样本进行分析。目标化合物采用外标曲线法进行定量。该方法线性范围为0.025.00 ng/ml,r = 0.999 9,方法检出限为0.002 ng/ml,定量限为0.02 ng/ml,加样回收率为89.60%98.60%。批内精密度为1.90%3.30%,批间精密度为4.20%9.00%;样本可在-20℃保存至少14天。样本中其他内源性物质对皮质醇的测定无干扰。该方法预处理简单,灵敏度高,重复性好,回收率高,适用于正常人群和职业应激人群唾液中皮质醇的定量分析。

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