Quantitative Analysis of Mevinolinic Acid in Human Plasma by High-performance Liquid Chromatography Coupled with Negative-ion Electrospray Tandem Mass Spectrometry

✍ Scribed by R. E. Calaf; M. Carrascal; E. Gelpí; J. Abian

• Publisher: John Wiley and Sons
• Year: 1997
• Tongue: English
• Weight: 136 KB
• Volume: 11
• Category: Article
• ISSN: 0951-4198
• DOI: 10.1002/(sici)1097-0231(19970115)11:1<75::aid-rcm797>3.0.co;2-3

✦ Synopsis

Mevinolinic acid (MVA), the major active metabolite of Lovastatin in human blood, is analysed by microbore high-performance liquid chromatography coupled to electrospray tandem mass spectrometry. Quantification is carried out by using methylmevinolinic acid (MMVA) as internal standard. Positive-and negative-ion mass spectra of these compounds are shown. Because of the higher sensitivity obtainable, the negative-ion mode is selected for the analysis. Solid-phase extraction cartridges are used off-line to prepurify and concentrate the sample and a microbore (1 × 100 mm) reversed-phase column is used for chromatography. Tandem mass spectrometry is carried out in the precursor-ion mode using a selected-reaction monitoring procedure. The [M-H] -precursor ions for MVA and MMVA are selected in the first quadrupole analyser and the second analyser is focused on the common product ion at m/z 319. Detection and quantification limits are ca. 50 pg/mL and ca. 200 pg/mL respectively. An example of the application of the method to the routine analysis of samples from a bioequivalence study is also shown.