LC-APCI-MS-MS methodology for determination of glybenclamide in human plasma
- 117 Downloads
A liquid chromatographic/atmospheric pressure chemical ionization tandem mass spectrometric method (LC-APCI-MS-MS) for the determination of glybenclamide in human plasma is described. Glypizide, an analogue of glybenclamide, was used as internal standard. The analyte was extracted from plasma with diethyl ether/dichloromethane (70:30 v/v). The chromatography uses C18 and 0.01 mol L−1 acetic acid/acetonitrile (20:80 v/v) as stationary and mobile phase, respectively. Quantitation was preformed by using multiple reaction monitoring (MRM) of the precursor ion (m/z 494.2→368.8) and the related product ion (m/z 446.0→347.3) using the internal standard method. The analytical curve was linear in the range 1–300 ng mL−1, and for a 400-μL sample of human plasma, the limit of determination of the method was 1 ng mL−1. The coefficients of variation of the method for intra-assay (within-run precision) and inter-assay (between-run precision) were less than 10%. The method was shown to be suitable for pharmacokinetic studies.
KeywordsGlybenclamide Sulfonylureas Plasma Mass spectrometry LC-APCI-MS-MS
The authors would like to acknowledge the technical assistance of Mr Jaime Ilha and the financial support of FAPESP (Grant No. 98/06007–5). M.R.L.M. thanks CAPES for a scholarship.
- 1.Al-Khamis KI, El-Sayed YM, Al-Rashood KA, Al-Yamani M (1994) Anal Lett 27:1277–1293Google Scholar
- 2.Sartor G, Lundquist I, Melander A, Scherstén B, Wahlin-Boll E (1982) J Clin Pharmacol 21:403–405Google Scholar
- 4.Santurio JRV, Porto EG (1996) J Chromatogr B 682:364–370Google Scholar
- 7.Sener A, Akkan AG, Malaisse WJ (1995) Acta Diabetologia 32:64–68Google Scholar
- 8.Susanto F, Reinauer H (1996) Fresenius J Anal Chem 356:352–357Google Scholar
- 9.Tiller PR, Land AP, Jardine I, Murphy DM, Sozio R, Ayrton A, Schaefer WH (1998) J Chromatogr A, 794:15–25Google Scholar
- 10.Ramos L, Bakhtiar R, Tse F (1999) Rapid Commun Mass Spectrom 13:2443Google Scholar
- 14.Moura MRL (2001) Konjac fiber: nutritional aspects and interaction with drug (glybenclamide). PhD thesis, College of Food Engineering, State University of Campinas, Brazil, p 88Google Scholar
- 15.Miller JC, Miller JN (1993) Statistics for analytical chemistry, 3rd edn. Ellis Horwood, p 233Google Scholar
- 17.Hsieh S, Selinger K (2002) J Chromatogr B 722:347–356Google Scholar