DEVELOPMENT AND VALIDATION OF STABILITY INDICATING GREEN HPLC-UV METHOD FOR DETERMINATION OF CEPHALEXIN IN PHARMACEUTICAL DOSAGE FORMS AND HUMAN URINE USING MICELLAR MOBILE PHASE

Authors

  • Ahmed Badr Eldin Sigma Pharmaceutical Industries, Quesna, Egypt
  • Omnia Ahmed Ismaiel Zagazig University
  • Waffa Hassan Zagazig University
  • Abdalla Shalaby Zagazig University

Keywords:

Green analytical chemistry, Cephalexin, Sodium dodecyl sulfate, Micelle L C, Human urine sample, Stability indicating method

Abstract

Objective: Development and validation of simple, stability indicating and green high performance liquid chromatographic (HPLC) method with ultraviolet (UV) detection for determination of cephalexin in pure form, pharmaceutical dosage forms and human urine samples.

Methods: The method is based on using of a micellar mobile phase for separation of cephalexin and its degradation products. The analyte was chromatographed on a Kinetex C18 75×4.6 mm, 2.6 μm column. Micellar mobile phase composed of 0.1M sodium dodecyl sulphate (SDS) and 10 % isopropanol (IPA), pH was adjusted to 3±0.05 with phosphoric acid, the flow-rate was 1.0 mL/min, the UV detector was set at 254 nm and the injection volume was 20 µl. Stability indicating properties of the proposed method was proved through exposure of the analyte solutions to 4 different stress conditions of acidic, basic, oxidative and photo-irradiation conditions.

Results: Under optimized conditions the average recovery was ranged from 100.4–101.7%. The lower limit of quantification (LOQ) and the lower limit of detection (LOD) were 0.097 and 0.029 μg/ml, respectively. A linear correlation in the range of 1–200 μg/ml with the correlation coefficient (r2) of ≥ 0.999 was obtained. Relatively high inter-and intra-day precisions were achieved, the percentage RSD values were lower than 2. The obtained results were validated according to USP validation parameters.

Conclusion: The proposed method was found to be not only a greener method but also faster and more convenient than the USP compendial method. Greener here means that the method is more eco-friendly as it avoids usage of toxic solvent and reagent and switch to more benign chemicals. In addition, allow for injection of urine samples directly into an analytical column without pretreatment due to micellar solubilization of the interfering components of the biological samples.

 

Downloads

Download data is not yet available.

References

Sittig M. Pharmaceutical Manufacturing Encyclopedia, Noyes, William Andrew Publishing, Park Ridge: New Jersey; 1988.

Garrigues S, S Armenta, M de la Guardia. Green strategies for decontamination of analytical wastes. TrAC Trends Anal Chem 2010:29;592-601.

Tanrisever B, P Santella. Cefadroxil. Drugs 1986;32:1-16.

Micronized F. United States Pharmacopoeia; 2012.

Najib N. High performance liquid chromatographic analysis of cephalexin in serum and urine. J Clin Pharm Ther 1987;12:419-26.

Zendelovska D, T Stafilov, S Petrov. Simultaneous quantification of cefaclor and cephalexine in blood plasma using high-performance liquid chromatography with UV detection. Acta Pharm Zagreb 2002;52:243-50.

Brogard J. Determination of cefalexin pharmacokinetics and dosage adjustments in relation to renal function. J Clin Pharmacol 1975;15:666-73.

Campíns-Falcó P. Comparative study on the determination of cephalexin in its dosage forms by spectrophotometry and HPLC with UV-vis detection. Microchim Acta 1997;126:207-15.

Al-Momani I. Spectrophotometric determination of selected cephalosporins in drug formulations using flow injection analysis. J Pharm Biomed Anal 2001;25:751-7.

Wu Z. Studies on the simultaneous measurement of several cephalosporins by RP-HPLC (I). Se pu= Chinese Journal of Chromatography/Zhongguo Hua Xue Hui 1999;17:518-21.

Rights IP, PM Power. Subject index to volumes. Atlanta 2010;2:713.

Marrelli L. Colorimetric estimation of cephalexin, cephaloglycin, and related compounds. J Pharm Sci 1972;61:1647-8.

Patel S, N Patel, M Patel. Spectrophotometric methods for the estimation of cephalexin in tablet dosage forms. Indian J Pharm Sci 2006;68:278.

Youngvises N. Greener liquid chromatography using a guard column with micellar mobile phase for separation of some pharmaceuticals and determination ofparabens. Talanta 2013;106:350-9.

El-Shaheny, RN, NM El-Enany, FF Belal. A green HPLC method for the analysis and stability study of flavoxate HCl using micellar eluent. Anal Methods 2014;6:1001-10.

Eldin AB. Applying green analytical chemistry (GAC) for development of stability indicating HPLC method for determining clonazepam and its related substances in pharmaceutical formulations and calculating uncertainty. Arabian J Chem 2014. doi:10.1016/j.arabjc.2014.10.051. [Article in Press]

Martindale W, SC Sweetman. Martindale: The complete drug reference: Pharmaceutical press London; 1999.

Van Deemter, JJ, F Zuiderweg, AV Klinkenberg. Longitudinal diffusion and resistance to mass transfer as causes of nonideality in chromatography. Chem Eng Sci 1956;5:271-89.

Khaledi MG. Micelles as separation media in high-performance liquid chromatography and high-performance capillary electrophoresis: overview and perspective. J Chromatogr A 1997;780:3-40.

Cho H. Statistical copolymers for blue-light-emitting diodes. Macromolecules 1999;32:1476-81.

Bahri P, P Tsintis. Pharmacovigilanceâ€related topics at the level of the International Conference on Harmonisation (ICH). Pharmacoepidemiol Drug Saf 2005;14:377-87.

Sittig M. Pharmaceutical Manufacturing Encyclopedia, Noyes, William Andrew Publishing, Park Ridge: New Jersey; 1988.

Heyden YV, Nijhuis A, Smeyers-Verbeke J, Vandeginste DL. Comparison of FT-NIR transmission and HPLC to assay montelukast in its pharmaceutical tablets. J Pharm Biomed Anal 2001;2:885-91.

Rapado Martínez I, Villanueva Camañas RM, García Alvarez-Coque MC. Micellar liquid chromatography: a worthy technique for the determination of β-antagonists in urine samples. Anal Chem 2009;71:319–26.

Published

01-09-2015

How to Cite

Eldin, A. B., O. A. Ismaiel, W. Hassan, and A. Shalaby. “DEVELOPMENT AND VALIDATION OF STABILITY INDICATING GREEN HPLC-UV METHOD FOR DETERMINATION OF CEPHALEXIN IN PHARMACEUTICAL DOSAGE FORMS AND HUMAN URINE USING MICELLAR MOBILE PHASE”. International Journal of Pharmacy and Pharmaceutical Sciences, vol. 7, no. 9, Sept. 2015, pp. 122-7, https://mail.innovareacademics.in/journals/index.php/ijpps/article/view/5950.

Issue

Section

Original Article(s)