二维手性色谱联用加速器质谱用于定量血浆中（14）C标记的R-和S-维拉帕米的方法开发。
Development of 2D chiral chromatography with accelerator mass spectrometry for quantification of (14)C-labeled R- and S-verapamil in plasma.
作者信息
Simpson M, Lappin G, Keely B J
机构信息
Xceleron Ltd, York, YO10 5NY, UK.
出版信息
Bioanalysis. 2010 Mar;2(3):397-405. doi: 10.4155/bio.10.7.
BACKGROUND
A microdose study was performed where 50 µg R/S-(14)C-verapamil was dosed intravenously to human volunteers. In order to quantify the individual R- and S-enantiomers in human plasma a 2D chiral HPLC method with subsequent analysis by accelerator mass spectrometry was verified.
RESULTS
R/S-verapamil was separated on a C18 column and the isolated fraction was applied to a chiral column where the verapamil enantiomers were separated. Experimental recovery (∼73% [coefficient of variation {CV} = 16%] and 66% [CV = 21%] for R- and S-verapamil, respectively) was accounted for by the use of internal standardization from the fluorescence response of nonlabeled R- and S-verapamil. The precision of the assay ranged from 4.1 to 15.9% CV and the limit of quantitation was 1.95-4.81 pg/ml for R-verapamil and 1.76-3.34 pg/ml for S-verapamil.
CONCLUSION
This method was successfully applied to the analysis of R- and S-verapamil in human plasma.
背景
进行了一项微剂量研究，向人类志愿者静脉注射50μg R/S-(14)C-维拉帕米。为了定量人血浆中的单个R-和S-对映体，验证了一种二维手性高效液相色谱法，随后通过加速器质谱进行分析。
结果
R/S-维拉帕米在C18柱上分离，分离出的馏分应用于手性柱，维拉帕米对映体在该柱上分离。通过使用来自未标记R-和S-维拉帕米荧光响应的内标法，实验回收率（R-维拉帕米分别为~73%[变异系数{CV}=16%]和S-维拉帕米为66%[CV=21%]）得以计算。该测定方法的精密度范围为CV的4.1%至15.9%，R-维拉帕米的定量限为1.95 - 4.81 pg/ml，S-维拉帕米的定量限为1.76 - 3.34 pg/ml。
结论
该方法成功应用于人血浆中R-和S-维拉帕米的分析。
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