Comparison of dried matrix spots and fabric phase sorptive extraction methods for quantification of highly potent analgesic activity agent (2R,4aR,7R,8aR)-4,7-dimethyl-2-(thiophen-2-yl)octahydro-2H-chromen-4-ol in rat whole blood and plasma using LC–MS/MS

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2019-11, Vol.1132, p.121813-121813, Article 121813
• Main Authors: Lastovka, Anastasiya V., Rogachev, Artem D., Il'ina, Irina V., Kabir, Abuzar, Volcho, Konstantin P., Fadeeva, Valentina P., Pokrovsky, Andrey G., Furton, Kenneth G., Salakhutdinov, Nariman F.
• Format: Article
• Language: English
• Subjects: (2R,4aR,7R,8aR)-4,7-dimethyl-2-(thiophen-2-yl)octahydro-2H-chromen-4-ol; Analgesic agent; Analgesics - blood; Animals; Benzopyrans - blood; Chromatography, Liquid - methods; Dried Blood Spot Testing - methods; Dried matrix spots; Fabric phase sorptive extraction; FPSE biofluid sampler; LC–MS/MS; Limit of Detection; Linear Models; Rats; Reproducibility of Results; Tandem Mass Spectrometry - methods; Thiophenes - blood
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2019.121813

•Dried blood spots, dried plasma spots and fabric phase sorptive extraction compared.•Fabric phase sorptive extraction provided better selectivity towards the target analyte.•FPSE disks demonstrate as a sustainable alternative to dried blood spot (DBS Cards). The methods for quantification of highly potent analgesic agent (2R,4aR,7R,8aR)-4,7-dimethyl-2-(thiophen-2-yl)octahydro-2H-chromen-4-ol in rat whole blood and plasma were developed and validated using dried matrix spots (DMS) or fabric phase sorptive extraction (FPSE) techniques in combination with LC–MS/MS. 2-Adamantylamine hydrochloride was used as an internal standard (IS). Chromatographic separation was carried out on a reversed-phase column (2.0×75 mm, 5 μm) using water containing 0.1% formic acid and methanol containing 0.1% formic acid as mobile phases in gradient mode at a flow rate of 200 μL/min. The mass spectrometric detection was performed using electrospray ionization (ESI) in positive ion mode. MRM transitions were m/z 284.5 → 137.2/157.4 for the analgesic agent and m/z 152.3 → 93.1/107.2 for IS. Calibration curves were linear within 20–5000 ng/mL in dried plasma spots (DPS) or dried blood spots (DBS) experiments. The linearity was obtained in the range of 20–5000 ng/mL and 50–5000 ng/mL for plasma-FPSE and blood-FPSE experiments, respectively. The intra- and inter-day accuracy and precision did not exceed acceptable limits. The mean extraction recovery (%) was 26 for DPS, 25 for DBS, 38 for plasma-FPSE, 31 for blood-FPSE.