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

1997; Wiley; Volume: 11; Issue: 1 Linguagem: Inglês

10.1002/(sici)1097-0231(19970115)11

1097-0231

Rosa E. Calaf, Montserrat Carrascal, E. Gelpı́, Joaquín Abián,

Pharmacological Effects and Assays

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. © 1997 John Wiley & Sons, Ltd.