High-performance liquid chromatography-tandem mass spectrometry for the analysis of bile acid profiles in serum of women with intrahepatic cholestasis of pregnancy

High-performance liquid chromatography-tandem mass spectrometry for the analysis of bile acid profiles in serum of women with intrahepatic cholestasis of pregnancy
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DOI:
10.1016/j.jchromb.2007.09.031
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发表时间:
2007-12-01
影响因子:
3
通讯作者:
Ding, Min
Ding, Min
中科院分区:
医学3区
文献类型:
--
作者:
Ye, Lian;Liu, Suya;Ding, Min

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一个简单的。建立了灵敏、特异的高效液相色谱-串联质谱(HPLC-MS/MS)分析胆汁酸谱的方法。采用HPLC-MS/MS对游离胆汁酸和共轭胆汁酸等15种胆汁酸进行分离和检测。采用负离子模式电喷雾电离(ESI)进行质谱检测。采用多反应监测(MRM)模式,采用外标曲线法定量。一个样品的总分析时间为15分钟,包括柱的再平衡时间。在0.02 ~ 100.0 μ mol/L范围内线性良好,各胆汁酸标准曲线相关系数均大于0.999。不同胆汁酸的检出限为0.001 ~ 0.006 μ mol/L。每种胆汁酸的精密度日内cv < 3.8%,日内cv < 6.1%。所有胆汁酸的平均加样回收率在86 ~ 110.0%之间。将该方法应用于53例健康妊娠妇女和43例妊娠肝内胆汁淤积症(ICP)妇女的临床样本分析。结果显示,胆汁酸谱在患有ICP的妇女和健康妊娠的妇女之间有显著差异。(C) 2007 Elsevier B.V.版权所有
A simple. sensitive, and specific high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the analysis of the bile acid profile has been developed. Fifteen bile acids, including free and conjugated bile acids, were separated and detected by HPLC-MS/MS. The MS detection was performed by electrospray ionization (ESI) in negative ion mode. Quantification was achieved in multiple reaction monitoring (MRM) mode with external standard curve methods. Total analysis time was 15 min for one sample including re-equilibration time of the column. The assay was linear in the range 0.02-100.0 mu mol/L with correlation coefficients of standard curves for all bile acids better than 0.999. The detection limits ranged from 0.001 to 0.006 mu mol/L for different bile acids. The precisions for each bile acid were CVs < 3.8% for within-day and CVs < 6.1% for between-day. The average recoveries for all bile acids studied were in the range of 86-110.0%. The developed method was applied to the analysis of clinic samples consisting of 53 women with healthy pregnancies and 43 women with intrahepatic cholestasis of pregnancy (ICP). The results revealed that the bile acid profile was markedly different between women with ICP and women with healthy pregnancies. (C) 2007 Elsevier B.V. All rights reserved.