Micro-SPE in pipette tips as a tool for analysis of small-molecule drugs in serum

Micro-SPE in pipette tips (μ-SPE-PT) with particle sorbent has never been used in small-molecule drug analysis. μ-SPE-PT was used for the extraction of statins from biological materials followed by UHPLC-MS/MS. The commercial and homemade μ-SPE-PT tips filled with particle sorbent were compared. Whi...

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Bibliographic Details
Published inBioanalysis Vol. 9; no. 11; pp. 887 - 901
Main Authors Vl ková, Hana, Pila ová, Veronika, Novák, Ond ej, Solich, Petr, Nováková, Lucie
Format Journal Article
LanguageEnglish
Published England Future Science Ltd 01.06.2017
Subjects
Chromatography, High Pressure Liquid - methods
Equipment Design
Humans
Limit of Detection
Pharmaceutical Preparations - blood
pipette tips
sample preparation
Solid Phase Microextraction - instrumentation
Solid Phase Microextraction - methods
statin
Tandem Mass Spectrometry - methods
UHPLC-MS/MS
μ-SPE-PT
UHPLC–MS/MS
statin
pipette tips
sample preparation
μ-SPE-PT
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Summary:Micro-SPE in pipette tips (μ-SPE-PT) with particle sorbent has never been used in small-molecule drug analysis. μ-SPE-PT was used for the extraction of statins from biological materials followed by UHPLC-MS/MS. The commercial and homemade μ-SPE-PT tips filled with particle sorbent were compared. While the homemade tips enabled direct serum sample loading into the sorbent, protein precipitation (PP) had to be implemented before μ-SPE-PT procedure using commercial tips. Three μ-SPE-PT methods were developed and validated: method A: μ-SPE-PT with homemade tips; method B: PP + μ-SPE-PT with homemade tips; and method C: PP + μ-SPE-PT with commercial tips. Method A enabled a simple high-throughput approach (48 samples in 90 min) compared with methods B and C that required three-times longer time. However, PP increased the recoveries of protein-bound analytes and extracts purity in methods B and C. The matrix effects without internal standards correction for method C were significantly higher than those for the methods A and B. Compared with commercial tips, homemade tips filled with particles were found to be more suitable for drug analysis. Commercial tips tested in this study were found challenging but the conditions under which they could be applicable were also defined.
ISSN:1757-6180
1757-6199
DOI:10.4155/bio-2017-0033