Using temperature to optimize resolution and reduce analysis times for bioanalytical diastereomer LC-MS/MS separations

被引：6

作者：

Cunliffe, Jennifer M. ^{[1
]}

Dreyer, Daniel P. ^{[1
]}

Hayes, Roger N. ^{[1
]}

Clement, Robert P. ^{[1
]}

Shen, Jim X. ^{[1
]}

机构：

[1] Merck Res Labs, Summit, NJ 07901 USA

来源：

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2011年 / 54卷 / 01期

关键词：

Bioanalytical; Diastereomer separations; High temperature HPLC; Resolution; PHASE LIQUID-CHROMATOGRAPHY; ULTRA-HIGH-PRESSURE; ELEVATED-TEMPERATURES; MASS-SPECTROMETRY; MOBILE PHASES; RETENTION; VALIDATION; PARTICLES; MOLECULES;

D O I：

10.1016/j.jpba.2010.08.017

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

A rugged and reproducible liquid chromatographic tandem mass spectrometric bioanalytical method was developed for the quantitation of drug stereoisomers in human plasma. Column temperature was shown to be an important variable toward optimizing diastereomer selectivity, resolution and analysis cycle time. Non-linear Van't Hoff plots and changes in peak shape with temperature suggested that selectivity was governed by multiple retention mechanisms. The high temperature chromatography method was validated and used to analyze samples from human clinical trials. Utilization of high temperature chromatography offered alternative selectivity and is a viable approach for difficult separations in regulated bioanalysis. (c) 2010 Elsevier B.V. All rights reserved.

引用

页码：179 / 185

页数：7

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