Abstract
A simple, selective, precise, and stability-indicating thin-layer chromatographic method has been developed and validated for analysis of the cephalosporins cefpodoxime proxetil, ceftriaxone sodium, ceftazidime pentahydrate, cefotaxime sodium, cefoperazone sodium, cefazolin sodium, and cefixime in the bulk drug and in pharmaceutical formulations. TLC was performed on aluminium sheets precoated with silica gel G 60F254 as stationary phase. The mobile phases chosen for development gave compact spots for all the drugs (R F values 0.43–0.60). The separated compounds were visualized as orange spots by spraying with Dragendorff’s reagent. Linear regression analysis data for the calibration plots revealed good linear relationships between response and amounts of the drugs with correlation coefficients ranging from 0.9977 to 0.9998 and determination coefficients ranging from 0.9954 to 0.9996 over the concentration ranges 5–25 μg per spot for cefpodoxime proxetil, ceftriaxone sodium, and ceftazidime pentahydrate and 10–50 μg per spot for cefotaxime sodium, cefoperazone sodium, cefazolin sodium, and cefixime. The method was validated for precision, recovery, and robustness. Limits of detection and quantitation for the drugs ranged from 0.35 to 2.48 and from 1.07 to 7.50 μg per spot, respectively. The method was successfully applied to analysis of the drugs in their pharmaceutical dosage forms with good precision and accuracy. The method can also be used as a stability-indicating assay.
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Delgaso JN, Remers WA (2004) Wilson and Gisvold’s textbook of organic medicinal and pharmaceutical chemistry, 10th edn. Lippincott Williams and Wilkins, New York
United States Pharmacopeia (2008) USP 31 and NF 26. American Pharmaceutical Association, Washington, DC
Ayad MM, Shalaby AA, Abdellatef HE, Elsaid HM (1999) J Pharm Biomed Anal 20:557–564. doi:10.1016/S0731-7085(99)00014-X
Rao GD, Kumar KG, Chowdary KPR (2001) Indian J Pharm Sci 63:161–163
Amin AS, Shama SA (2000) Monatsh Chem 131:313–319. doi:10.1007/s007060050312
Salem H (2004) Anal Chim Acta 515:333–341. doi:10.1016/j.aca.2004.03.056
Kumar KG, Chowdary KPR, Rao GD (2001) Antiseptic 98:149–150
El-Walily AFM, Gazy AA, Belal SF, Khamis EF (2000) Spectrosc Lett 33:931–948. doi:10.1080/00387010009350169
Yang J, Zhou GJ, Cao XH, Ma QL, Dong J (1998) Anal Lett 31:1047–1060
Yang JH, Ma QL, Wu X, Sun LM, Cao XH (1999) Anal Lett 32:471–480. doi:10.1080/00032719908542834
El-Maali NA, Ali AMM, Ghandour MA (1993) Electroanalysis 5:599–604. doi:10.1002/elan.1140050712
Ferreira VS, Zanoni MVB, Fogg AG (1999) Anal Chim Acta 384:159–166. doi:10.1016/S0003-2670(98)00813-7
Yılmaz N, Biryol I (1998) J Pharm Biomed Anal 17:1335–1344. doi:10.1016/S0731-7085(98)00040-5
Ferreira VS, Zanoni MVB, Fogg AG (1998) Anal Chim Acta 367:255–259. doi:10.1016/S0003-2670(98)00163-9
Misztal G (1998) Pharmazie 53:723–724
Shinde VM, Shabadi CV (1998) Indian J Pharm Sci 60:313–315
Barnes AR (1995) J Liq Chromatogr 18:3117–3128. doi:10.1080/10826079508010437
Robbitt JM (1963) Thin-layer chromatography. Chapman and Hall, London
Qureshi SZ, Jamhour RMAQ, Rahman N (1996) J Planar Chromatogr 9:466–469
Kelani K, Bebawy LI, Abdel-Fattah L (1998) J AOAC Int 81:386–393
Dhanesar SC (1998) J Planar Chromatogr 11:195–200
Dhanesar SC (1999) J Planar Chromatogr 12:114–119
Zarapkar SS, Shivalkar SA, Dhanvate AA, Deshpande PM, Kolte SS (1995) Indian Drugs 32:232–235
Gupta MM, Verma RK (1996) Indian J Pharm Sci 58:161–162
Szabó B, Lakatos A, Kõszegi T, Kátay G, Botz L (2005) J AOAC Int 88:1571–1577
Tyrpień K, Bodzek P, Mańka G (2001) Biomed Chromatogr 15:50–55. doi:10.1002/bmc.36
Moffat MC, Jackson JV, Moss MS, Widdop B, Greefield ES (1986) Clarke’s isolation and identification of drugs, 2nd edn. The Pharmaceutical Press, London, pp 133, 142 and 1169
International Conference on Harmonization (2005) Topic Q2 (R1): validation of analytical procedures: text and methodology. http://www.ich.org/LOB/media/MEDIA417.pdf
Pedersen O (2006) Pharmaceutical chemical analysis: methods for identification and limit tests. CRC Press, Taylor and Francis, New York, pp 16–17
Heyden YV, Nijhuis A, Smeyers-Verbeke J, Vandeginste BGM, Massart DL (2004) J Pharm Biomed Anal 24:723–753. doi:10.1016/S0731-7085(00)00529-X
International Conference on Harmonization (2003) Guidance for industry, Q1A (R2): stability testing of new drug substances and products. IFPMA, Geneva. http://www.fda.gov/cber/gdlns/ichstab.htm
Saleh GA, Askal H, Darwish I, El-Shorbagi A (2003) Anal Sci 19:281–287. doi:10.2116/analsci.19.281
Rodriguez LC, Gracia LG, Loèpez EMA, Sendra JMB (2001) Trends Analyt Chem 20:620–636. doi:10.1016/S0165-9936(01)00111-X
Harvey D (2000) Modern analytical chemistry. McGraw–Hill, Boston, MA, pp 108 and 622
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Mohamed, F.A., Saleh, G.A., El-Shaboury, S.R. et al. Selective Densitometric Analysis of Cephalosporins Using Dragendorff’s Reagent. Chroma 68, 365–374 (2008). https://doi.org/10.1365/s10337-008-0714-3
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DOI: https://doi.org/10.1365/s10337-008-0714-3