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Quantitative determination of α‐cyclodextrin in human plasma by liquid chromatography/positive ion electrospray mass spectrometry
Author(s) -
Hammes Wilhelm,
Bourscheidt Christine,
Büchsler Ursula,
Stodt Gabi,
Bökens Hilmar
Publication year - 2000
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/(sici)1096-9888(200003)35:3<378::aid-jms945>3.0.co;2-m
Subject(s) - chemistry , chromatography , protein precipitation , electrospray ionization , mass spectrometry , analyte , detection limit , electrospray , calibration curve , perchloric acid , solid phase extraction , selected reaction monitoring , analytical chemistry (journal) , extraction (chemistry) , tandem mass spectrometry , organic chemistry
A sensitive and selective method for the determination of α‐cyclodextrin in human plasma is described using β‐cyclodextrin as an internal standard. After protein precipitation with perchloric acid, the analytes were isolated from human plasma by solid‐phase extraction on Bond Elut C 18 cartridges. The compounds were chromatographed on a narrow‐bore aminopropyl column (125 × 2 mm i.d., 5 µm) and analyzed by electrospray ionization mass spectrometry in the positive selected‐ion mode using the [M + NH 4 ] + ion. The lower limit of quantitation was 5 ng ml −1 of human plasma. Linear calibration curves were obtained over the concentration range 5–1000 ng ml −1 of human plasma. The intra‐ and inter‐assay precisions were <18% and the accuracy was <10.5% over the entire concentration range. During the method development, the ionization efficiencies of the analytes in plasma samples originating from different sources were examined to overcome the matrix effect problems caused by co‐eluting endogenous compounds. The method was successfully applied to pharmacokinetic studies in human volunteers. Copyright © 2000 John Wiley & Sons, Ltd.