Micellar HPLC Method for Simultaneous Determination of Ethamsylate and Mefenamic Acid in Presence of Their Main Impurities and Degradation Products.
An eco-friendly sensitive, rapid and less hazardous micellar liquid chromatographic method was developed and validated for the simultaneous analysis of ethamsylate (ETM) and mefenamic acid (MFA) in the presence of hydroquinone (HQ) and 2,3-dimethylaniline (DMA) the main impurities of ETM and MFA, respectively. Good chromatographic separation was attained using Eclipse XDB-C8 column (150 mm × 4.6 mm, 5 μm particle size) adopting UV detection at 300 nm with micellar mobile phase consisting of 0.12 M sodium dodecyl sulfate, 0.3% triethylamine and 15% 2-propanol in 0.02 M orthophosphoric acid (pH 7.0) at 1.0 mL/min. The analytes were well resolved in <6.0 min, ETM (tR= 1.55 min), HQ (tR= 1.95 min), MFA (tR= 4.55 min) and DMA (tR= 5.80 min). Different validation parameters were examined as recommended by international conference on harmonization (ICH) guidelines. The method was linear over the concentration ranges of 0.5-18.0, 0.5-20.0, 0.01-0.5 and 0.02-0.2 µg/mL with limits of detection of 0.118, 0.159, 0.005 and 0.005 µg/mL and limits of quantification of 0.358, 0.482, 0.014 and 0.015 µg/mL for ETM, MFA, HQ and DMA, respectively. The suggested method was successfully applied for the determination of the two drugs in their bulk powder, laboratory-prepared mixtures, single-ingredient and co-formulated tablets. The obtained results were in accordance with those of the comparison method. The method can also detect trace amounts of HQ and DMA as the main impurities of ETM and MFA, respectively, within the BP limit (0.1%) for both impurities. Furthermore, it is a stability-indicating one for the determination of ETM in its pure form, single-component tablet and co-formulated tablets with other drugs.
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Fawzia
F
Ibrahim
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Mohie K
MK
Sharaf El-Din
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.|Department of Agro-Environmental Sciences, Graduate School of Bioresource and Bioenviromental Sciences, Kyushu University, Fukuoka 812-8581, Japan.
Asmaa Kamal
AK
El-Deen
Department of Agro-Environmental Sciences, Graduate School of Bioresource and Bioenviromental Sciences, Kyushu University, Fukuoka 812-8581, Japan shimizu@agr.kyushu-u.ac.jp.
Kuniyoshi
K
Shimizu
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004979:Ethamsylate / Q000032:analysis* / Q000737:chemistry; D057230:Limit of Detection; D016014:Linear Models; D008528:Mefenamic Acid / Q000032:analysis* / Q000737:chemistry; D008823:Micelles; D015203:Reproducibility of Results
D008823:Micelles; D004979:Ethamsylate; D008528:Mefenamic Acid