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The application of fast gradient capillary liquid chromatography/mass spectrometry to the analysis of pharmaceuticals in biofluids
Author(s) -
Plumb R. S.,
Dear G. J.,
Mallett D.,
Fraser I. J.,
Ayrton J.,
Ioannou C.
Publication year - 1999
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/(sici)1097-0231(19990530)13:10<865::aid-rcm570>3.0.co;2-0
Subject(s) - chemistry , chromatography , capillary action , bioanalysis , mass spectrometry , high performance liquid chromatography , reproducibility , gradient elution , elution , protein precipitation , analytical chemistry (journal) , materials science , composite material
Fast gradient capillary high performance liquid chromatography (HPLC) coupled to a mass spectrometer has been successfully used for the analysis of pharmaceutical compounds from biological matrices, in the femtogram on column range. In the work reported in this paper, the use of capillary HPLC, on the 180‐µm internal diameter scale, has shown a 30‐fold improvement in detection limits when compared to conventional 2‐mm scale chromatography. The use of fast gradient elution resulted in a generic methodology which gave excellent chromatographic reproducibility and column longevity. This technique has been used in conjunction with simple protein precipitation, with no deleterious effect on either the column life or the chromatographic performance. The use of capillary HPLC in bioanalysis has the potential to give a significant increase in assay sensitivity with the equipment currently in use. In this paper the authors also present a modification to the current PE‐Sciex ion‐spray source which allows excellent spray adjustment in three dimensional accessibility, which is important when working with low flow rates, as well as reducing the inherent system dead volume. Copyright © 1999 John Wiley & Sons, Ltd.