A RAPID UHPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF SELECTED B-BLOCKERS, NSAIDS, AND THEIR METABOLITES IN HUMAN URINE AND WATER SAMPLES

Abstract

A rapid Ultra High Performance Liquid Chromatography (UHPLC) method for the simultaneous determination of β-blockers (sotalol SOT, metoprolol MET, propranolol PRO), Non-steroidal Anti-inflammatory Drugs (NSAIDs) (paracetamol PAR, ketoprofen KET, salicylic acid SAL), and their metabolites (paracetamol sulfate PAR-S, paracetamol glucuronide PAR-G, ketoprofen glucuronide KET-G, o-desmethylmetoprolol D-MET, α-hydroxymetoprolol MET-H, 4′-hydroxypropranolol sulphate PRO-S) is presented in this paper. The separation of twelve determined substances was conducted by means of a C₁₈ Fast Gradient monolithic column (50 mm × 2 mm) in no longer than 7.5 min. The amounts of analytes introduced onto the column varied from 0.09 ng to 0.69 ng in a 1-μL injection. The method was validated for the determination of these substances in human urine and tap water, according to Solid Phase Extraction (SPE) procedures. The linearity ranges for the analyzed substances were (μg/mL): 0.60–40 for PAR-G; 0.69–44 for PAR-S; 0.60–42 for PAR; 0.33–40 for SOT; 0.30–35 for MET-H; 0.27–40 for DMET; 0.40–45 for SAL; 0.33–40 for PRO-S; 0.40–36 for MET; 0.45–42 for PRO, 0.36–46 for KET, and for 0.42–40 KET-G. The described method was successfully applied to water samples and to urine from patients who were administered the aforementioned drugs.

Keywords:

• beta blockers
• drugs
• metabolites
• NSAIDs
• solid phase extraction
• UHPLC-UV

ACKNOWLEDGMENTS

We would like to thank Merck (Poland) for use of their LaChrom Ultra HPLC equipment.

This work was partially supported by funds for scientific research for 2007–2010 as Research Developmental Project No. 017670.

Notes

^a Calculated with ChemAxon Marvin Calculator.

^a Standard deviation of a slope.

^b Standard deviation of intercept.

^a blank human urine extracted on C₁₈ cartridges.