Sensitive determination of aspirin and its metabolites in plasma by LC–UV using on-line solid-phase extraction with methylcellulose-immobilized anion-exchange restricted access media

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 846; no. 1; pp. 132 - 138
• Main Authors: Yamamoto, Eiichi, Takakuwa, Susumu, Kato, Takashi, Asakawa, Naoki
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 01.02.2007; Elsevier Science
• Subjects: Analysis; Analytical, structural and metabolic biochemistry; Animals; Anion Exchange Resins; Anion-exchanger; Aspirin; Aspirin - blood; Aspirin - pharmacokinetics; Biological and medical sciences; Chromatography, Ion Exchange - methods; Fundamental and applied biological sciences. Psychology; General pharmacology; Male; Medical sciences; Methylcellulose - chemistry; Pharmacokinetics; Pharmacology. Drug treatments; Plasma; Rats; Rats, Sprague-Dawley; Reproducibility of Results; Restricted-access media; Sensitivity and Specificity; Solid-phase extraction; Spectrophotometry, Ultraviolet - methods; Plasma; Anion-exchanger; Aspirin; Restricted-access media; Pharmacokinetics; Solid-phase extraction; Prostaglandin-endoperoxide synthase; Solid phase extraction; Biological fluid; Metabolite; Immobilization; Laxative; Acetylsalicylic acid; Determination; Blood plasma; Anion exchange; Salicylates; Quantitative analysis; Restricted access medium column; Enzyme; Enzyme inhibitor; Antiplatelet agent; Non steroidal antiinflammatory agent; Methylcellulose; Analgesic; Antipyretic; Anion exchanger; Oxidoreductases
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2006.08.037

We describe a sensitive determination of aspirin (ASA) and its three metabolites (salicylic acid [SA], 2,3-dihydroxybenzoic acid [2,3-DHBA], and 2,5-dihydroxybenzoic acid [gentisic acid (GA)]) in rat plasma. Analysis was carried out by on-line solid-phase extraction (SPE) using a methylcellulose-immobilized-strong anion-exchanger (MC-SAX), followed by liquid chromatography (LC) coupled with UV detection. The lower limits of quantitation for ASA and SA were 60 ng/mL in 100 μL of plasma, respectively. This method was validated with respect to intra- and inter-day precision, accuracy, and linearity up to concentrations of 20,000 ng/mL for ASA, SA, 2,3-DHBA and gentisic acid, respectively. The method was successfully applied to an analysis of the pharmacokinetics of ASA and SA in rats.