Revised sample preparation for the analysis of oxysterols by enzyme-assisted derivatisation for sterol analysis (EADSA).
Revised sample preparation for the analysis of oxysterols by enzyme-assisted derivatisation for sterol analysis (EADSA).
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DOI：
10.1007/s00216-015-8609-2
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发表时间：
2015-07
影响因子：
4.3
通讯作者：
Griffiths, William J.
中科院分区：
文献类型：
--
作者：
Crick, Peter J.;Bentley, T. William;Wang, Yuqin;Griffiths, William J.
关键词：
甾醇，特别是氧甾醇，在胆汁酸和类固醇激素的生物合成中起重要作用，并且本身具有生物活性。氧固醇的分析是复杂的，由于其在生物系统中的低丰度和差的质谱电离特性。在过去的十年中，我们已经开发了一种液相色谱-质谱法称为酶辅助衍生甾醇分析（EADSA）。我们的衍生化程序依赖于两个固相萃取步骤，以（i）将胆固醇与氧固醇分离，以及（ii）去除过量的衍生化试剂。最近C18反相柱的批间变化导致我们使用替代柱进行实验。在这里，我们提出了我们的研究结果，并报告了一种改进的样品制备程序，使用聚合物亲油平衡反相柱。本文的在线版本（doi：10.1007/s 00216 -015-8609-2）包含补充材料，可供授权用户使用。
Sterols, and specifically oxysterols, play important roles in the biosynthesis of bile acids and steroid hormones as well as possessing biological activities in their own right. Analysis of oxysterols is complicated due to their low abundance in biological systems and poor ionisation characteristics in mass spectrometry. Over the past decade, we have developed a liquid chromatography–mass spectrometry method termed enzyme-assisted derivatisation for sterol analysis (EADSA). Our derivatisation procedure relies on two solid-phase extraction steps to (i) separate cholesterol from oxysterols and (ii) remove excess derivatisation reagents. Recent inter-batch variation in C18 reversed-phase cartridges has led us to experiment with alternative columns. Here, we present our findings and report an improved sample preparation procedure using polymeric hydrophilic–lipophilic balanced reversed-phase cartridges. The online version of this article (doi:10.1007/s00216-015-8609-2) contains supplementary material, which is available to authorized users.
影响因子：
2.9
作者：
DZELETOVIC, S;BREUER, O;DICZFALUSY, U
通讯作者：
DICZFALUSY, U
影响因子：
6.5
作者：
McDonald, Jeffrey G.;Smith, Daniel D.;Russell, David W.
通讯作者：
Russell, David W.
影响因子：
7.4
作者：
Griffiths, William J.;Crick, Peter J.;Wang, Yuqin
通讯作者：
Wang, Yuqin