PMID- 17481971 OWN - NLM STAT- MEDLINE DCOM- 20071009 LR - 20191210 IS - 1570-0232 (Print) IS - 1570-0232 (Linking) VI - 854 IP - 1-2 DP - 2007 Jul 1 TI - Validation of a rapid micellar electrokinetic capillary chromatographic method for the simultaneous determination of isoniazid and pyridoxine hydrochloride in pharmaceutical formulation. PG - 35-42 AB - An efficient and reliable micellar electrokinetic capillary chromatography (MEKC) method has been developed for the simultaneous determination of isoniazid (ISO) and pyridoxine hydrochloride (PYR) in pharmaceutical formulations. A chemometric two level full factorial design approach was used to search for the optimum conditions of separation. Three parameters were selected for this study: the buffer pH, the buffer concentration and sodium dodecyl sulphate (SDS) concentrations. Resolution, peak symmetry and analysis time were established as response. The two analytes were separated within 6 min with the optimized conditions: 50 mM borate buffer, 25 mM SDS pH 7.8, 35 degrees C, at 50 mbar 4s injection and 30 kV by using a fused silica capillary (72 cm effective length, 50 microm i.d.). The detection wavelength was set to 205 nm. Meloxicam was used as internal standard. The method was validated with respect to stability, linearity range, limit of quantitation and detection, precision, accuracy, specificity and robustness. The detection limits of the method were 1.0 microg mL(-1) for ISO and 0.40 microg mL(-1) for PYR and the method was linear at least in the range of 3.0-100 microg mL(-1) for ISO and 1.0-100 microg mL(-1) for PYR with excellent correlation coefficients (0.9995 for ISO and 0.9998 for PYR). Relative standard deviations (R.S.D.s) of the described method ranged between 0.54 and 2.27% for intra-day precision and between 0.65 and 2.69% for inter-day precision. The developed method was applied to the tablet form of ISO and PYR-containing the pharmaceutical preparations and the data were compared with obtained from the standard addition method. No statistically significant difference was found. FAU - Nemutlu, E AU - Nemutlu E AD - Department of Analytical Chemistry, Faculty of Pharmacy, University of Hacettepe, 06100 Ankara, Turkey. FAU - Celebier, M AU - Celebier M FAU - Uyar, B AU - Uyar B FAU - Altinoz, S AU - Altinoz S LA - eng PT - Journal Article PT - Validation Study DEP - 20070412 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Pharmaceutical Preparations) RN - KV2JZ1BI6Z (Pyridoxine) RN - V83O1VOZ8L (Isoniazid) SB - IM MH - Chromatography, Micellar Electrokinetic Capillary/*methods MH - Isoniazid/*analysis MH - Pharmaceutical Preparations/*chemistry MH - Pyridoxine/*analysis MH - Reproducibility of Results MH - Sensitivity and Specificity EDAT- 2007/05/08 09:00 MHDA- 2007/10/10 09:00 CRDT- 2007/05/08 09:00 PHST- 2006/11/15 00:00 [received] PHST- 2007/03/09 00:00 [revised] PHST- 2007/03/26 00:00 [accepted] PHST- 2007/05/08 09:00 [pubmed] PHST- 2007/10/10 09:00 [medline] PHST- 2007/05/08 09:00 [entrez] AID - S1570-0232(07)00256-5 [pii] AID - 10.1016/j.jchromb.2007.03.050 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jul 1;854(1-2):35-42. doi: 10.1016/j.jchromb.2007.03.050. Epub 2007 Apr 12.