Development of a thin-film solid-phase microextraction (TF-SPME) method coupled to liquid chromatography and tandem mass
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RESEARCH PAPER
Development of a thin-film solid-phase microextraction (TF-SPME) method coupled to liquid chromatography and tandem mass spectrometry for high-throughput determination of steroid hormones in white sucker fish plasma Małgorzata Maciążek-Jurczyk 1,2 & Vincent Bessonneau 1 & Jennifer Ings 3 & Leslie Bragg 4 & Mark McMaster 3 & Mark R. Servos 4 & Barbara Bojko 1,5 & Janusz Pawliszyn 1 Received: 31 January 2020 / Revised: 28 March 2020 / Accepted: 9 April 2020 # Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract Steroid hormones (SH) play a number of important physiological roles in vertebrates including fish. Changes in SH concentration significantly affect reproduction, differentiation, development, or metabolism. The objective of this study was to develop an in vitro high-throughput thin-film solid-phase microextraction (TF-SPME)–liquid chromatography– tandem mass spectrometry (LC–MS/MS) method for targeted analysis of endogenous SH (cortisol, testosterone, progesterone, estrone (E1), 17β-estradiol (E2), and 17α-ethinylestradiol (EE2)) in wild white sucker fish plasma where the concentrations of the analytes are substantially low. A simple TF-SPME method enabled the simultaneous determination of free and total SH concentrations. The use of biocompatible coating allowed direct extraction of these hormones from complex biological samples without prior preparation. The carryover was less than 3%, thereby ensuring reusability of the devices and reproducibility. The results showed that TF-SPME was suitable for the analysis of compounds in the polarity range between 1.28 and 4.31 such as SH at different physicochemical properties. The proposed method was validated according to bioanalytical method validation guidelines. The limit of detection (LOD) and limit of quantification(LOQ) for cortisol, testosterone, progesterone, E1, E2, and EE2 were from 0.006 to 0.150 ng/mL and from 0.020 to 0.500 ng/mL, respectively. The recovery for the method was about 85%, and the accuracy and precision of the method for cortisol, testosterone, and progesterone were ≤ 6.0% and ≤ 11.2%, respectively, whereas those for E1, E2, and EE2 were ≤ 15.0% and ≤ 10.2%, respectively. On the basis of this study, TFSPME demonstrated several important advantages such as simplicity, sensitivity, and robustness under laboratory conditions.
Keywords Thin-film solid-phase microextraction . Thin-film coated blades . Fish steroid hormones . LC–MS/MS
Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02657-x) contains supplementary material, which is available to authorized users. * Janusz Pawliszyn [email protected] 1
Department of Chemistry, University of Waterloo, Waterloo, Ontario N2L 3G1, Canada
2
Department of Physical Pharmacy, Faculty of Pharmaceutical Sciences in Sosnowiec, Medical University of Silesia in Katowice, 41-200 Sosnowiec, Poland
3
Enviroment and Climate Change Canada, Burlington, Ontario L7S 1A1, Canada
4
Department of Biology, University of Wat
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