Mass-directed fractionation and isolation of pharmaceutical compounds by packed-column supercritical fluid chromatography/mass spectrometry

被引:46
作者
Wang, T [1 ]
Barber, M [1 ]
Hardt, I [1 ]
Kassel, DB [1 ]
机构
[1] DuPont Pharmaceut Res Labs, San Diego, CA 92121 USA
关键词
D O I
10.1002/rcm.480
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
An automated packed-column semi-preparative supercritical fluid chromatography/mass spectrometry (SFC/MS) system incorporating mass-directed fraction collection has been designed and implemented as an alternative to preparative HPLC and preparative HPLC/MS (PrepLC/MS) for the purification of pharmaceutical compounds. The system incorporates a single quadrupole mass spectrometer and a supercritical fluid chromatograph. Separations were achieved using a binary solvent system consisting of carbon dioxide and methanol. Purification of SFC-separated compounds was achieved incorporating mass-directed fraction collection, enabling selective isolation of the target molecular weight compound and eliminating the collection of undesired compounds (e.g., by-products, excess starting materials, etc.). Cross contamination between fractions and recoveries of the system were investigated. Mass spectrometer ionization with basic mobile additives is discussed, and examples of preparative SFC/MS chiral separations are presented. Early experiences suggest SFC will be a powerful and complementary technique to HPLC for the purification of pharmaceutical compounds. Copyright (C) 2001 John Wiley & Sons, Ltd.
引用
收藏
页码:2067 / 2075
页数:9
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