Pharmaceutical Analysis Laboratory, Biological and Medical Research Department (MBC-03), King Faisal Specialist Hospital and Research Centre, P.O. Box 3354, Riyadh 1211, Saudi Arabia.
Talanta. 2003 Dec 4;61(5):667-73. doi: 10.1016/S0039-9140(03)00352-7.
A new analytical method for the separation and determination of R-(-)- and S-(+)- baclofen enantiomers in human plasma by high-performance liquid chromatography (HPLC) with UV detection was developed. Enantioselective resolution of the baclofen enantiomers was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with a polar ionic mobile phase (PIM) consisting of methanol: glacial acetic acid: triethylamine, 100:0.1:0.1, (v/v/v) at a flow rate of 0.5 ml min(-1) and UV detection set at 220 nm. The analytes of interest with S-(+)-sulpiride as the internal standard were extracted from human plasma using liquid-liquid extraction procedure with ethyl ether under alkaline condition prior to HPLC analysis. Recoveries for R-(-)- and S-(+)-baclofen enantiomers were in the ranges of 96-103% at 60-2500 ng ml(-1) level. Intra-day and inter-day precision calculated as %RSD was in the ranges of 1.2-5.2 and 1.3-4.3% for both enantiomers, respectively. Intra-day and inter-day accuracy calculated as percentage error were in the ranges of 1.2-3.9 and 1.1-3.9% for both enantiomers, respectively. Linear calibration curves in the concentration ranges of 20-3000 ng ml(-1) for each enantiomer showed correlation coefficient (r) of 0.9997. The limit of quantitation (LOQ) and limit of detection (LOD) for each enantiomer in human plasma were 20 and 10 ng ml(-1) (S/N=3) respectively.
建立了一种新的分析方法，用于通过高效液相色谱（HPLC）与紫外检测法分离和测定人血浆中的 R-（-）-和 S-（+）-巴氯芬对映体。通过使用已知为 Chirobiotic T 的泰乐菌素大环抗生素手性固定相（CSP），并使用包含甲醇：冰醋酸：三乙胺的极性离子流动相（PIM），实现了巴氯芬对映体的对映选择性拆分，甲醇：冰醋酸：三乙胺，100：0.1：0.1，（v/v/v），流速为 0.5 ml min（-1），紫外检测波长设定为 220nm。在 HPLC 分析之前，用碱性条件下的乙醚进行液-液萃取，将感兴趣的分析物与 S-（+）-舒必利作为内标从人血浆中提取出来。R-（-）-和 S-（+）-巴氯芬对映体的回收率在 60-2500ng ml（-1）水平范围内为 96-103%。两种对映体的日内和日间精密度（以%RSD 计算）分别在 1.2-5.2 和 1.3-4.3%的范围内。两种对映体的日内和日间准确度（以百分比误差计算）分别在 1.2-3.9 和 1.1-3.9%的范围内。每个对映体的浓度范围为 20-3000ng ml（-1）的线性校准曲线的相关系数（r）为 0.9997。两种对映体在人血浆中的定量限（LOQ）和检测限（LOD）分别为 20 和 10ng ml（-1）（S/N=3）。
