Article

Quantitative determination of fluvastatin in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry using [18O2]-fluvastatin as an internal standard.

University Children's Hospital, Division of Analytical Biochemistry and Mass Spectrometry, Auenbruggerplatz 30, A-8036 Graz, Austria.
Rapid Communications in Mass Spectrometry (impact factor: 2.79). 02/2005; 19(2):128-32. DOI:10.1002/rcm.1758 pp.128-32
Source: PubMed

ABSTRACT A sensitive and specific method for the quantitative determination of fluvastatin in human plasma is presented. The drug was isolated from plasma by extractive alkylation with pentafluorobenzyl bromide and further derivatized to the bis-trimethylsilyl derivative. [18O2]-Fluvastatin was prepared from unlabelled fluvastatin and used as an internal standard. Gas chromatography/mass spectrometry under negative ion chemical ionization conditions was used for quantitative measurement of the drug, using m/z 554.26 and 558.26 for target and internal standard, respectively. Calibration graphs were linear within a range of 2 and 512 ng mL(-1) plasma. Intra-day precision was 0.94% (2 ng mL(-1)), 2.53% (8.2 ng mL(-1)), 2.16% (81.9 ng mL(-1)) and 3.26% (409.6 ng mL(-1)); inter-day variability was found to be 1.64% (2 ng mL(-1)), 0.97% (8.2 ng mL(-1)), 1.97% (81.9 ng mL(-1)) and 2.01% (409.6 ng mL(-1)). Intra-day accuracy showed deviations of 0.6% (2 ng mL(-1)), 0.37% (8.2 ng mL(-1)), -1.52% (81.9 ng mL(-1)) and -1.67% (409.6 ng mL(-1)); inter-day accuracy was of -1.64% (2 ng mL(-1)), -1.13% (8.2 ng mL(-1)), -2.28% (81.9 ng mL(-1)) and -0.46% (409.6 ng mL(-1)). The stable isotope labelled standard was found to be stable under the analytical conditions.

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Keywords

analytical conditions
 
bis-trimethylsilyl derivative
 
derivatized
 
fluvastatin
 
Gas chromatography/mass spectrometry
 
human plasma
 
Intra-day precision
 
negative ion chemical ionization conditions
 
pentafluorobenzyl bromide
 
plasma
 
quantitative determination
 
quantitative measurement
 
specific method
 
unlabelled fluvastatin