Microextraction by packed sorbent and high performance liquid chromatography determination of seven non-steroidal anti-inflammatory drugs in human plasma and urine

• Published in: Journal of Chromatography A Vol. 1367; pp. 1 - 8
• Main Authors: Locatelli, Marcello, Ferrone, Vincenzo, Cifelli, Roberta, Barbacane, Renato Carmine, Carlucci, Giuseppe
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 07.11.2014; Elsevier
• Subjects: Analysis; Analytical chemistry; Anti-Inflammatory Agents, Non-Steroidal - blood; Anti-Inflammatory Agents, Non-Steroidal - urine; Biological and medical sciences; Calibration; Chromatography, High Pressure Liquid - methods; General pharmacology; High performance liquid chromatography; Human; Human plasma; Human urine; Humans; Ibuprofen; indomethacin; ketoprofen; Limit of Detection; Linearity; Medical sciences; MEPS-HPLC-PDA; Method development; microextraction; Nonsteroidal antiinflammatory drugs; NSAIDs; particle size; Pharmacology. Drug treatments; Sample preparation; Solid Phase Microextraction - methods; sorbents; Urine; Human plasma; Sample preparation; Method development; NSAIDs; Human urine; MEPS-HPLC-PDA; Biological fluid; Chemical analysis; HPLC chromatography; Blood; Chemical enrichment; Blood plasma; Diode array; Quantitative analysis; Trace analysis; Human; Urine; Validation; Fluorescence detector; Elution; Gradient; Healthy subject; Elimination; Non steroidal antiinflammatory agent; Solid phase microextraction; Reversed phase chromatography; Ultraviolet detector; Syringe
• DOI: 10.1016/j.chroma.2014.09.034
• ISSN: 0021-9673

•First MEPS-HPLC–PDA assay for NSAIDs analysis in plasma and urine.•Simultaneous determination of seven NSAIDs in biological matrices.•The method can be adopted for rapid multi-components analyses in biological matrix.•Validation procedure fulfilling ICH Q2(R1) guidelines. This paper reports a new MEPS-HPLC-PDA method for the simultaneous analysis of seven non-steroidal anti-inflammatory drugs (Furprofen, Indoprofen, Ketoprofen, Fenbufen, Flurbiprofen, Indomethacin, and Ibuprofen) in human plasma and urine. NSAIDs were resolved on a Gemini C18 column (4.6mm×250mm; 5μm particle size) using a gradient elution mode with a run time of 25min, comprising re-equilibration, without further purification. The method was validated over the concentration range from 0.1 to 10μg/mL for all the analytes both in human plasma and urine, using Benzyl 4-hydroxybenzoate as the internal standards. This method was successfully tested to NSAIDs analyses in real matrices, in order to check the method potentiality and the correct response. The results from assay validations show that the method is selective, sensitive and robust. The limit of quantification of the method was 0.1μg/mL for all analytes, and weighted-matrix-matched standard curves showed a good linearity up to 10μg/mL. In order to check the correct response for over-range samples, parallelism tests were also assessed. In the entire analytical range the intra and inter-day precision (RSD%) values were ≤7.31% and ≤13.5%, respectively. For all the analytes the intra and inter-day trueness (Bias%) values ranged from −11.3% to 10.2%. To our knowledge, this is the first MEPS-HPLC-PDA based method that uses MEPS procedure for simultaneous determination of these seven NSAIDs in plasma and urine samples.