Pharma / Biotech

UHPLC assisted simultaneous separation of apigenin and prednisolone and its application in the pharmacokinetics of apigenin.

Icon for Elsevier Science Related Articles

UHPLC assisted simultaneous separation of apigenin and prednisolone and its application in the pharmacokinetics of apigenin.

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Apr 03;1117:58-65

Authors: Elzayat EM, Shakeel F, Alshehri S, Ibrahim MA, Altamimi MA, Kazi M, Alanazi FK, Haq N

A new ultra-high performance liquid chromatography-mass spectrometry-mass spectrometry (UHPLC-MS/MS) system has been formulated for the resolution of closely related drugs apigenin (API, a bioflavinoid) and prednisolone (PRD) from their mixture. This developed method comprised of a “BEH™ C18 column (50 mm × 2.1 mm, 1.7 μm)” using acetonitrile and 0.1% formic acid (35:65 v/v) at a supply rate of 0.25 mL·min-1 as eluent. It was found that selected eluent provided short run time (≤2.5 min) as well as better peak symmetry. Satisfactory values of chromatographic parameters such as resolution (Rs = 2.5), capacity factor (k; 13.6 and 23.4 for API and PRD respectively, selectivity (α = 1.72) and number of theoretical plates (N; 3789 and 42,435 for API and PRD respectively) indicate the efficiency of the developed method. The obtained separation was then exploited for the detection and measurement of API in rat plasma sample by means of PRD as an “internal standard” (IS). The eluted compounds in plasma were identified by tandem mass spectrometry by means of tandem quadrupole (TQ) detector (“Waters Corp., Milford, MA”) fortified with an “electrospray ionisation (ESI)” source functioning in positive ionization mode. The determination of API in plasma was accomplished by means of “multiple reactions monitoring (MRM)” mode. Assortment of “ionization pairs” (m/z) was displayed in the following manner: API: 270.99 → 152.9 (“cone voltage” 57 V, “collision energy” 34 V), PRD: 403.172 → 385.224 (“cone voltage” 42 V, “collision energy” 13 V). The calibration curves followed linearity in concentration range of 05-1000 ng mL-1 with limit of detection “LOD” and limit of quantification “LOQ” of 7.30 and 22.77 ng mL-1, respectively. The developed method was validated taking into consideration various test conditions and satisfactory values of various parameters such as linearity (r2 ± SD = 0.9995 ± 0.0005), interday accuracy (88-120%), interday precision % RSD = 3.30-13.65% whereas intraday accuracy (91-118%) intraday precision % RSD = 1.18-5.83) indicated its validity. The validation outcomes fulfilled the standards of united states food and drug administration “USFDA” in addition Scientific Working Group for Forensic Toxicology “SWGTOX” guiding principles and were not beyond the tolerable constraint. The process developed in plasma was efficaciously harnessed in the pharmacokinetic investigation of various formulations of API after oral administration in rats.

PMID: 30999274 [PubMed – as supplied by publisher]

Source link

Related posts

FDA Approves Nubeqa to Treat Prostate Cancer


Investigation of MDR1-overexpressing cell lines to derive a quantitative prediction approach for brain disposition using in vitro efflux activities.


Extra-endothelial TRPV1 channels participate in alcohol and caffeine actions on cerebral artery diameter.


This website uses cookies to improve your experience. We'll assume you're ok with this, but you can opt-out if you wish. Accept Read More

Privacy & Cookies Policy