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Mass‐directed fractionation and isolation of pharmaceutical compounds by packed‐column supercritical fluid chromatography/mass spectrometry
Author(s) -
Wang Tao,
Barber Michael,
Hardt Ingo,
Kassel Daniel B.
Publication year - 2001
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.480
Subject(s) - chemistry , chromatography , mass spectrometry , fractionation , supercritical fluid chromatography , packed bed , supercritical fluid , isolation (microbiology) , column (typography) , column chromatography , organic chemistry , connection (principal bundle) , structural engineering , microbiology and biotechnology , biology , engineering
Abstract 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 © 2001 John Wiley & Sons, Ltd.