Simultaneous determination of procaine and para-aminobenzoic acid by LC–MS/MS method

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 847; no. 2; pp. 224 - 230
• Main Authors: Dhananjeyan, Mugunthu R., Bykowski, Crystal, Trendel, Jill A., Sarver, Jeffrey G., Ando, Howard, Erhardt, Paul W.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 01.03.2007; Elsevier Science
• Subjects: 4-Aminobenzoic Acid - analysis; 4-Aminobenzoic Acid - chemistry; Analysis; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Chromatography, High Pressure Liquid - methods; Diseases of the skin. Cosmetics; Esters; Fundamental and applied biological sciences. Psychology; General pharmacology; LC–MS/MS; Local anesthetics; Medical sciences; Molecular Structure; NAPA; PABA; Pharmacology. Drug treatments; Procaine; Procaine - analysis; Procaine - chemistry; Radiotherapy. Instrumental treatment. Physiotherapy. Reeducation. Rehabilitation, orthophony, crenotherapy. Diet therapy and various other treatments (general aspects); Reproducibility of Results; Tandem Mass Spectrometry - methods; NAPA; Esters; Procaine; PABA; LC–MS/MS; Local anesthetics; Chemical analysis; Liquid chromatography; Local anesthetic; Aminobenzoic acid; Ester; LC-MS/MS; Simultaneous measurement; Sunscreen product
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2006.10.004

A sensitive high performance liquid chromatography tandem mass spectrometry (LC–MS/MS) method has been developed for simultaneous determination of procaine and its metabolite p-aminobenzoic acid (PABA). N-Acetylprocainamide (NAPA) was used as an internal standard for procaine and PABA analysis. This assay method has also been validated in terms of linearity, lower limit of detection, lower limit of quantitation, accuracy and precision as per ICH guidelines. Chromatography was carried out on an XTerra™ MS C 18 column and mass spectrometric analysis was performed using a Quattro Micro™ mass spectrometer working with electro-spray ionization (ESI) source in the positive ion mode. Enhanced selectivity was achieved using multiple reaction monitoring (MRM) functions, m/ z 237 → 100, m/ z 138 → 120, and m/ z 278 → 205 for procaine, PABA and NAPA, respectively. Retention times for PABA, procaine and NAPA were 4.0, 4.7 and 5.8 min, respectively. Linearity for each calibration curve was observed across a range from 100 nM to 5000 nM for PABA, and from 10 nM to 5000 nM for procaine. The intra- and inter-day relative standard deviations (RSD) were <5%.