title: Microextraction by packed sorbent as sample preparation step for atorvastatin and its metabolites in biological samples--critical evaluation.
abstract: Atorvastatin belongs to the group of lipid-lowering drugs known as statins. They significantly reduce the levels of total cholesterol, low-density cholesterol and plasma triglycerides therefore they are widely used in the treatment of hypercholesterolemia. Recently developed methods for the determination of atorvastatin and its metabolites in plasma used SPE (solid phase extraction) or LLE (liquid-liquid extraction) as the sample preparation step. However, both procedures are quite time-consuming and need relatively high volume of solvent/sample, which is impractical for the routine analyses of many biological samples. The aim of this work was to develop and validate more suitable sample preparation method for the determination of atorvastatin and its metabolites in biological samples using MEPS (microextraction by packed sorbent). The optimal conditions of MEPS extraction were using C8 sorbent and only 50 μl of the sample. The analytes were eluted by 100 μl of the mixture of acetonitrile:0.1 M ammonium acetate pH 4.5 (95:5, v:v). The analytical method was validated and demonstrated good linearity (r(2)>0.9990), recovery (89-115%) and intra-day precision (RSD<10%). Total time of the sample preparation was three times shorter (7 min) compared to SPE. The volume of sample was twenty times lower and the volume of solvents about ten times lower compared to SPE. Combination of fast MEPS method together with quick UHPLC-MS/MS was used for the determination of atorvastatin and its two metabolites in serum obtained from patients with familiar hypercholesterolemia.
authors.affiliation: Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Medical School and Teaching Hospital, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
authors.forename: Hana
authors.initials: H
authors.lastname: Vlčková
authors.forename: Dagmar
authors.initials: D
authors.lastname: Solichová
authors.forename: Milan
authors.initials: M
authors.lastname: Bláha
authors.forename: Petr
authors.initials: P
authors.lastname: Solich
authors.forename: Lucie
authors.initials: L
authors.lastname: Nováková
mesh_terms: D000924:Anticholesteremic Agents / Q000302:isolation & purification* / Q000378:metabolism; D000069059:Atorvastatin; D002784:Cholesterol / Q000097:blood; D006538:Heptanoic Acids / Q000302:isolation & purification* / Q000378:metabolism; D006801:Humans; D019161:Hydroxymethylglutaryl-CoA Reductase Inhibitors / Q000302:isolation & purification* / Q000378:metabolism; D011758:Pyrroles / Q000302:isolation & purification* / Q000378:metabolism; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D014280:Triglycerides / Q000097:blood
chemical_list: D000924:Anticholesteremic Agents; D006538:Heptanoic Acids; D019161:Hydroxymethylglutaryl-CoA Reductase Inhibitors; D011758:Pyrroles; D014280:Triglycerides; D002784:Cholesterol; D000069059:Atorvastatin