Determination of methyl and ethyl esters of methanesulfonic, benzenesulfonic and p-toluenesulfonic acids in active pharmaceutical ingredients by solid-phase microextraction (SPME) coupled to GC/SIM-MS

• Published in: Journal of pharmaceutical and biomedical analysis Vol. 39; no. 3; pp. 477 - 485
• Main Authors: Colón, Ivelisse, Richoll, Stephen M.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 15-09-2005; Elsevier Science
• Subjects: Active pharmaceutical ingredients; Analysis; Analytical, structural and metabolic biochemistry; Benzenesulfonates - chemistry; Biological and medical sciences; Chemistry, Pharmaceutical - methods; Chromatography; Chromatography, Gas - methods; Drug Industry - methods; Esters - chemistry; Fundamental and applied biological sciences. Psychology; Gas Chromatography-Mass Spectrometry; General pharmacology; Hydrogen-Ion Concentration; Impurity analysis; LPME; Medical sciences; Mesylates - chemistry; Pharmacology. Drug treatments; Phosphates - chemistry; Reproducibility of Results; Sensitivity and Specificity; Solid-phase microextraction; SPE; SPME; Sulfonate esters; Sulfonic acid esters; Time Factors; SPME; Sulfonate esters; Impurity analysis; Solid-phase microextraction; Sulfonic acid esters; SPE; Active pharmaceutical ingredients; LPME; Solid phase extraction; Impurity; Solid phase microextraction; Active ingredient; Quantitative analysis
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2005.04.037

The development, optimization and validation of an extraction method for methyl and ethyl esters of various sulfonic acids is presented. The extraction and determination of these esters in active pharmaceutical ingredients (APIs) was accomplished using solid-phase microextraction coupled to GC/MS in the SIM mode. The factors affecting the extraction efficiency are discussed. This method was validated as a limits test and allows the determination of the sulfonic esters at the 5
ppm level in APIs. The method proved to be reproducible (%R.S.D.s less than 6%) and suitable for use with external standard quantitation, and also met basic validation requirements. This method offers numerous advantages over liquid–liquid extraction methods and was also compared to other extraction techniques such as solid-phase extraction (SPE) and liquid-phase microextraction (LPME) also being developed in our laboratories.