Rapid Method for Analysis of Aspirin-Butalbital in Serum Utilizing a Monolithic C18 Column

• Published in: Journal of liquid chromatography & related technologies Vol. 26; no. 15; pp. 2567 - 2579
• Main Authors: Pistos, C., Stewart, J. T.
• Format: Journal Article
• Language: English
• Published: Colchester Taylor & Francis Group 01.08.2003; Taylor & Francis
• Subjects: Analysis; Aspirin-butalbital mixture; Biological and medical sciences; column; General pharmacology; HPLC; Human serum; Medical sciences; Monolithic C; Pharmacology. Drug treatments; Human; Solid phase extraction; Biological fluid; Chemical analysis; Monolithic column; HPLC chromatography; Hypnotic; Acetylsalicylic acid; Blood; Non steroidal antiinflammatory agent; Butalbital; Reversed phase chromatography; Analgesic; Ultraviolet detector; Sample preparation; Simultaneous measurement; Antipyretic; Salicylates; Sedative; Barbiturates; Blood serum; Quantitative analysis
• ISSN: 1082-6076; 1520-572X
• DOI: 10.1081/JLC-120023801

A fast and sensitive high performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of aspirin-butalbital in human serum. Serum samples were treated with a solid phase extraction procedure. The analytes were separated using a mobile phase of 90:10 (v/v) 0.1 M aqueous potassium phosphate monobasic (pH 4)-acetonitrile on a monolithic C 18 column with UV detection at 220 nm. Benzoic acid was used as the internal standard (IS). The method was validated over the range of 0.5-100 µg mL −1 for each drug. The method proved to be accurate (percent bias for all calibration samples varied from −13 to 6.6%) and precise (range from 0.1% to 10%). The mean percent absolute recoveries were 104 ± 6.3 for aspirin, 92.6 ± 5.5 for butalbital and 106 ± 6.9 for the internal standard. The assay should be applicable for use in pharmacokinetic studies and routine serum monitoring of these drugs.