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Separation and determination of nimesulide related substances for quality control purposes by micellar electrokinetic chromatography.
J Pharm Biomed Anal. 2009 Feb 20; 49(2):201-6.JP

Abstract

A micellar electrokinetic chromatography (MEKC) method has been developed and validated for the determination of nimesulide related compounds in pharmaceutical formulations. Electrophoretic separation of six European Pharmacopoeia (EP) impurities (A-F) was performed using a fused silica capillary (L(eff.)=50 cm, L(tot.)=57 cm, 50 microm i.d.) with a background electrolyte (BGE) containing 25 mM borate buffer (pH 9.5), 30 mM sodium dodecyl sulphate and phi=3% (v/v) acetonitrile. The influence of several factors (surfactant and buffer concentration, pH, organic modifier, applied voltage, capillary temperature and injection time) was studied. The method was suitably validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. The calibration curves obtained for the six compounds were linear over the range 5-12 microgml(-1) (0.05-0.12%). The relative standard deviations (s(r)) of intra- and inter-day experiments were less than 5.0%. The detection limits ranged between 0.7 and 1.6 microgml(-1) depending on the impurity. The proposed method was applied successfully to the quantification of nimesulide impurities in its pharmaceutical formulation.

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Authors+Show Affiliations

Zacharis CK
Department of Chemistry, Aristotle University, GR-54124 Thessaloniki, Greece.
Tzanavaras PD
No affiliation info available
Notou M
No affiliation info available
Zotou A
No affiliation info available
Themelis DG
No affiliation info available

MeSH

Anti-Inflammatory Agents, Non-SteroidalBoric AcidsBuffersCalibrationChromatography, Micellar Electrokinetic CapillaryDrug ContaminationElectricityElectrolytesHydrogen-Ion ConcentrationMolecular StructurePharmaceutical PreparationsPharmacopoeias as TopicQuality ControlReproducibility of ResultsSensitivity and SpecificitySodium Dodecyl SulfateSulfonamidesSurface-Active AgentsTabletsTemperature

Pub Type(s)

Journal Article

Language

eng

PubMed ID

19062217

Citation

Zacharis, Constantinos K., et al. "Separation and Determination of Nimesulide Related Substances for Quality Control Purposes By Micellar Electrokinetic Chromatography." Journal of Pharmaceutical and Biomedical Analysis, vol. 49, no. 2, 2009, pp. 201-6.
Zacharis CK, Tzanavaras PD, Notou M, et al. Separation and determination of nimesulide related substances for quality control purposes by micellar electrokinetic chromatography. J Pharm Biomed Anal. 2009;49(2):201-6.
Zacharis, C. K., Tzanavaras, P. D., Notou, M., Zotou, A., & Themelis, D. G. (2009). Separation and determination of nimesulide related substances for quality control purposes by micellar electrokinetic chromatography. Journal of Pharmaceutical and Biomedical Analysis, 49(2), 201-6. https://doi.org/10.1016/j.jpba.2008.10.023
Zacharis CK, et al. Separation and Determination of Nimesulide Related Substances for Quality Control Purposes By Micellar Electrokinetic Chromatography. J Pharm Biomed Anal. 2009 Feb 20;49(2):201-6. PubMed PMID: 19062217.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Separation and determination of nimesulide related substances for quality control purposes by micellar electrokinetic chromatography. AU - Zacharis,Constantinos K, AU - Tzanavaras,Paraskevas D, AU - Notou,Maria, AU - Zotou,Anastasia, AU - Themelis,Demetrius G, Y1 - 2008/10/28/ PY - 2008/09/23/received PY - 2008/10/15/revised PY - 2008/10/17/accepted PY - 2008/12/9/pubmed PY - 2009/5/1/medline PY - 2008/12/9/entrez SP - 201 EP - 6 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 49 IS - 2 N2 - A micellar electrokinetic chromatography (MEKC) method has been developed and validated for the determination of nimesulide related compounds in pharmaceutical formulations. Electrophoretic separation of six European Pharmacopoeia (EP) impurities (A-F) was performed using a fused silica capillary (L(eff.)=50 cm, L(tot.)=57 cm, 50 microm i.d.) with a background electrolyte (BGE) containing 25 mM borate buffer (pH 9.5), 30 mM sodium dodecyl sulphate and phi=3% (v/v) acetonitrile. The influence of several factors (surfactant and buffer concentration, pH, organic modifier, applied voltage, capillary temperature and injection time) was studied. The method was suitably validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. The calibration curves obtained for the six compounds were linear over the range 5-12 microgml(-1) (0.05-0.12%). The relative standard deviations (s(r)) of intra- and inter-day experiments were less than 5.0%. The detection limits ranged between 0.7 and 1.6 microgml(-1) depending on the impurity. The proposed method was applied successfully to the quantification of nimesulide impurities in its pharmaceutical formulation. SN - 0731-7085 UR - https://www.unboundmedicine.com/medline/citation/19062217/Separation_and_determination_of_nimesulide_related_substances_for_quality_control_purposes_by_micellar_electrokinetic_chromatography_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(08)00588-8 DB - PRIME DP - Unbound Medicine ER -