Merck Research Laboratories, 181 Passaic Avenue, Summit, NJ 07901, USA.
J Pharm Biomed Anal. 2011 Jan 5;54(1):179-85. doi: 10.1016/j.jpba.2010.08.017. Epub 2010 Aug 22.
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.
本研究建立了一种重现性好的用于定量分析人血浆中药物对映异构体的液相色谱-串联质谱分析方法。柱温是优化非对映异构体选择性、分辨率和分析周期时间的重要变量。非线性格林菲尔德图和温度变化对峰形的影响表明，选择性受多种保留机制控制。该高温色谱方法经过验证后，用于分析来自人体临床试验的样品。高温色谱的应用提供了替代选择性，是法规生物分析中困难分离的可行方法。
