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The effect of organic solvents on the determination of cyclic boronates of some β‐blockers by gas chromatography/mass spectrometry
Author(s) -
Lee JeongAe,
Lho Dongseok,
Kim Myungsoo,
Kim Keon,
Kim Yunje
Publication year - 1998
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(19980915)12:17<1150::aid-rcm282>3.0.co;2-5
Subject(s) - chemistry , chromatography , mass spectrometry , gas chromatography–mass spectrometry , gas chromatography , thermospray , tandem mass spectrometry , selected reaction monitoring
Formation cyclic boronates for β‐blockers, by use of triethylamine (TEA) and pyridine as catalysts, gives more effective product yield. Eleven β‐blockers, formed by cyclic boronation with n ‐butylboronic acid and TEA, produced higher yields than by on‐column thermal reaction and seven β‐blockers were shown to give the highest yields in the phenyl cyclic boronation with pyridine or TEA by on‐column thermal and general reaction. The phenyl cyclic boronate of nadolol produced one peak in the chromatogram and the n ‐butyl cyclic boronate showed two peaks. On‐column derivatization with n ‐butylboronic acid and pyridine was effective in saving analysis time and for convenience, even though some n ‐butyl cyclic boronates by cyclic boronation with TEA gave a better yield. In n ‐butyl cyclic boronation with pyridine by on‐column thermal reaction the detection limits were 0.1 to 4 ng/μL in urine with a signal‐to‐noise ratio of 10:1. © 1998 John Wiley & Sons, Ltd.