An improved and fully validated LC-MS/MS method for the simultaneous quantification of simvastatin and simvastatin acid in human plasma

Journal of Pharmaceutical and Biomedical Analysis
Constantinos ApostolouYannis L Loukas

Abstract

A fully automated high-throughput liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous quantification of simvastatin (SV) and simvastatin acid (SVA) in human plasma. Plasma samples were treated by acetonitrile (ACN) addition for protein precipitation (PP) and subsequent two-step liquid-liquid extraction (LLE) in 96-deepwell plates, using methyl t-butyl ether (MTBE) as the organic solvent. ACN addition step was proven to enhance method sensitivity, as well as producing cleaner samples for injection. Lovastatin (LV) and lovastatin acid (LVA) were used as internal standards (IS) for SV and SVA quantification respectively. A relatively small plasma volume (300 microL) was employed and all procedure liquid transfer steps were performed automatically, by the use of robotic liquid handling workstations. Both electrospray (ESI) and atmospheric pressure chemical ionization (APCI) sources were applied and compared for LC-MS/MS sample analysis, with ESI proven to be more sensitive for the specific analytes. Polarity switch (from negative to positive ionization mode) was performed during the same analytical run, so as for the simultaneous SV and SVA determination to be possible. The method had...Continue Reading

Citations

Dec 25, 2013·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Vinicius Freire FagundesChristian Fernandes
Jan 16, 2014·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Hilary J BewsCharles S Wong
Dec 19, 2013·European Journal of Drug Metabolism and Pharmacokinetics·Xiao-lin WangHui-chen Liu
Aug 22, 2009·British Journal of Clinical Pharmacology·Jenni E KeskitaloMikko Niemi
Nov 9, 2010·International Journal of Pharmaceutics·Francesca UngaroMaria Immacolata La Rotonda
Jun 22, 2017·Biochemical Pharmacology·Chun-Han LinChun-Jung Lin
Mar 27, 2018·Expert Review of Respiratory Medicine·Amir A Zeki, Mona Elbadawi-Sidhu
May 29, 2015·Pharmacogenetics and Genomics·Aleksi TornioMikko Niemi

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