Institute of Legal Medicine, University Medical Centre, Albertstr. 9, 79104 Freiburg, Germany.
Anal Bioanal Chem. 2010 Apr;396(7):2415-23. doi: 10.1007/s00216-010-3458-5. Epub 2010 Feb 2.
Phosphatidylethanol (PEth) is an abnormal phospholipid carrying two fatty acid chains. It is only formed in the presence of ethanol via the action of phospholipase D (PLD). Its use as a biomarker for alcohol consumption is currently under investigation. Previous methods for the analysis of PEth included high-performance liquid chromatography (HPLC) coupled to an evaporative light scattering detector (ELSD), which is unspecific for the different homologues--improved methods are now based on time of flight mass spectrometry (TOF-MS) and tandem mass spectrometry (MS/MS). The intention of this work was to identify as many homologues of PEth as possible. A screening procedure using multiple-reaction monitoring (MRM) for the identified homologues has subsequently been established. For our investigations, autopsy blood samples collected from heavy drinkers were used. Phosphatidylpropanol 16:0/18:1 (internal standard) was added to the blood samples prior to liquid-liquid extraction using borate buffer (pH 9), 2-propanol and n-hexane. After evaporation, the samples were redissolved in the mobile phase and injected into the LC-MS/MS system. Compounds were separated on a Luna Phenyl Hexyl column (50 mm x 2 mm, 3 microm) by gradient elution, using 2 mM ammonium acetate and methanol/acetone (95/5; v/v). A total of 48 homologues of PEth could be identified by using precursor ion and enhanced product ion scans (EPI).
磷脂酰乙醇(PEth)是一种异常的磷脂,带有两条脂肪酸链。它仅在乙醇存在下通过磷脂酶 D(PLD)的作用形成。目前正在研究将其用作酒精消耗的生物标志物。以前分析 PEth 的方法包括高效液相色谱(HPLC)与蒸发光散射检测器(ELSD)联用,该方法对不同同系物不具有特异性 - 现在改进的方法基于飞行时间质谱(TOF-MS)和串联质谱(MS/MS)。这项工作的目的是尽可能多地鉴定 PEth 的同系物。随后建立了使用多重反应监测(MRM)对鉴定出的同系物进行筛选的程序。在我们的研究中,使用来自重度饮酒者的尸检血液样本。在使用硼酸盐缓冲液(pH 9)、2-丙醇和正己烷进行液 - 液萃取之前,将磷脂酰丙醇 16:0/18:1(内标)添加到血液样本中。蒸发后,将样品重新溶解在流动相中,并注入 LC-MS/MS 系统。通过梯度洗脱,在 Luna Phenyl Hexyl 柱(50mm x 2mm,3μm)上分离化合物,使用 2mM 乙酸铵和甲醇/丙酮(95/5;v/v)。通过前体离子和增强产物离子扫描(EPI)可以鉴定出 48 种 PEth 同系物。