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Validated chromatographic methods for simultaneous determination of tolfenamic acid and its major impurities.
J Chromatogr Sci 2015; 53(4):484-91JC

Abstract

Two accurate, selective and precise chromatographic methods, namely thin-layer chromatography (TLC)-densitometric method and reversed phase high-performance liquid chromatography (RP-HPLC) method, were developed and validated for the simultaneous determination of tolfenamic acid (TOL) and its two major impurities, 2-chlorobenzoic acid (CBA) and 3-chloro-2-methylaniline (CMA), which are also reported to be its related substances. The developed TLC-densitometric method depended on separation and quantitation of the studied drugs on silica gel 60F254 TLC plates. Hexane:chloroform:acetone:acetic acid (75:25:20:0.1, v/v/v/v) was used as a developing system and the separated bands were UV-scanned at 240 nm. Linear relationships were obtained in the range of 10-100 µg band(-1) for the drug and in the range of 0.1-1 µg band(-1) for the studied impurities. The developed RP-HPLC depended on chromatographic separation of the studied drugs on a C18 column using 0.05 M KH2PO4 buffer (pH 3):acetonitrile (45:55, v/v) as a mobile phase delivered at constant flow rate of 1 mL min(-1) with UV detection at 230 nm. Calibration curves for TOL and the two impurities were constructed over the concentration ranges of 10-100 µg mL(-1) for TOL and 0.01-0.1 µg mL(-1) for both CBA and CMA. Factors affecting the developed methods have been studied and optimized. Further, methods validation has been carried out according to International Conference on Harmonization guidelines. The proposed methods were successfully applied for determination of the studied drug in its bulk powder and in pharmaceutical formulation. The methods showed no significant difference when compared with the reported RP-HPLC one. The developed methods have advantages of being more sensitive and specific than the published methods.

Authors+Show Affiliations

Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, Alshaheed Shehata Ahmed Hegazy St. Beni-Suef 62514, Egypt.Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, Alshaheed Shehata Ahmed Hegazy St. Beni-Suef 62514, Egypt.Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, Alshaheed Shehata Ahmed Hegazy St. Beni-Suef 62514, Egypt marcomounir11@yahoo.com.Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St, Cairo 11562, Egypt.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

25016532

Citation

Abdelwahab, Nada S., et al. "Validated Chromatographic Methods for Simultaneous Determination of Tolfenamic Acid and Its Major Impurities." Journal of Chromatographic Science, vol. 53, no. 4, 2015, pp. 484-91.
Abdelwahab NS, Ali NW, Zaki MM, et al. Validated chromatographic methods for simultaneous determination of tolfenamic acid and its major impurities. J Chromatogr Sci. 2015;53(4):484-91.
Abdelwahab, N. S., Ali, N. W., Zaki, M. M., & Abdelkawy, M. (2015). Validated chromatographic methods for simultaneous determination of tolfenamic acid and its major impurities. Journal of Chromatographic Science, 53(4), pp. 484-91. doi:10.1093/chromsci/bmu071.
Abdelwahab NS, et al. Validated Chromatographic Methods for Simultaneous Determination of Tolfenamic Acid and Its Major Impurities. J Chromatogr Sci. 2015;53(4):484-91. PubMed PMID: 25016532.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Validated chromatographic methods for simultaneous determination of tolfenamic acid and its major impurities. AU - Abdelwahab,Nada S, AU - Ali,Nouruddin W, AU - Zaki,Marco M, AU - Abdelkawy,M, Y1 - 2014/07/12/ PY - 2014/7/14/entrez PY - 2014/7/14/pubmed PY - 2015/12/15/medline SP - 484 EP - 91 JF - Journal of chromatographic science JO - J Chromatogr Sci VL - 53 IS - 4 N2 - Two accurate, selective and precise chromatographic methods, namely thin-layer chromatography (TLC)-densitometric method and reversed phase high-performance liquid chromatography (RP-HPLC) method, were developed and validated for the simultaneous determination of tolfenamic acid (TOL) and its two major impurities, 2-chlorobenzoic acid (CBA) and 3-chloro-2-methylaniline (CMA), which are also reported to be its related substances. The developed TLC-densitometric method depended on separation and quantitation of the studied drugs on silica gel 60F254 TLC plates. Hexane:chloroform:acetone:acetic acid (75:25:20:0.1, v/v/v/v) was used as a developing system and the separated bands were UV-scanned at 240 nm. Linear relationships were obtained in the range of 10-100 µg band(-1) for the drug and in the range of 0.1-1 µg band(-1) for the studied impurities. The developed RP-HPLC depended on chromatographic separation of the studied drugs on a C18 column using 0.05 M KH2PO4 buffer (pH 3):acetonitrile (45:55, v/v) as a mobile phase delivered at constant flow rate of 1 mL min(-1) with UV detection at 230 nm. Calibration curves for TOL and the two impurities were constructed over the concentration ranges of 10-100 µg mL(-1) for TOL and 0.01-0.1 µg mL(-1) for both CBA and CMA. Factors affecting the developed methods have been studied and optimized. Further, methods validation has been carried out according to International Conference on Harmonization guidelines. The proposed methods were successfully applied for determination of the studied drug in its bulk powder and in pharmaceutical formulation. The methods showed no significant difference when compared with the reported RP-HPLC one. The developed methods have advantages of being more sensitive and specific than the published methods. SN - 1945-239X UR - https://www.unboundmedicine.com/medline/citation/25016532/Validated_chromatographic_methods_for_simultaneous_determination_of_tolfenamic_acid_and_its_major_impurities_ L2 - https://academic.oup.com/chromsci/article-lookup/doi/10.1093/chromsci/bmu071 DB - PRIME DP - Unbound Medicine ER -