Skip to main content
Log in

Selective Densitometric Analysis of Cephalosporins Using Dragendorff’s Reagent

  • Original
  • Published:
Chromatographia Aims and scope Submit manuscript

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.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. Delgaso JN, Remers WA (2004) Wilson and Gisvold’s textbook of organic medicinal and pharmaceutical chemistry, 10th edn. Lippincott Williams and Wilkins, New York

    Google Scholar 

  2. United States Pharmacopeia (2008) USP 31 and NF 26. American Pharmaceutical Association, Washington, DC

  3. Ayad MM, Shalaby AA, Abdellatef HE, Elsaid HM (1999) J Pharm Biomed Anal 20:557–564. doi:10.1016/S0731-7085(99)00014-X

    Article  CAS  Google Scholar 

  4. Rao GD, Kumar KG, Chowdary KPR (2001) Indian J Pharm Sci 63:161–163

    Google Scholar 

  5. Amin AS, Shama SA (2000) Monatsh Chem 131:313–319. doi:10.1007/s007060050312

    Article  CAS  Google Scholar 

  6. Salem H (2004) Anal Chim Acta 515:333–341. doi:10.1016/j.aca.2004.03.056

    Article  CAS  Google Scholar 

  7. Kumar KG, Chowdary KPR, Rao GD (2001) Antiseptic 98:149–150

    Google Scholar 

  8. El-Walily AFM, Gazy AA, Belal SF, Khamis EF (2000) Spectrosc Lett 33:931–948. doi:10.1080/00387010009350169

    Article  CAS  Google Scholar 

  9. Yang J, Zhou GJ, Cao XH, Ma QL, Dong J (1998) Anal Lett 31:1047–1060

    CAS  Google Scholar 

  10. Yang JH, Ma QL, Wu X, Sun LM, Cao XH (1999) Anal Lett 32:471–480. doi:10.1080/00032719908542834

    Article  CAS  Google Scholar 

  11. El-Maali NA, Ali AMM, Ghandour MA (1993) Electroanalysis 5:599–604. doi:10.1002/elan.1140050712

    Article  CAS  Google Scholar 

  12. Ferreira VS, Zanoni MVB, Fogg AG (1999) Anal Chim Acta 384:159–166. doi:10.1016/S0003-2670(98)00813-7

    Article  CAS  Google Scholar 

  13. Yılmaz N, Biryol I (1998) J Pharm Biomed Anal 17:1335–1344. doi:10.1016/S0731-7085(98)00040-5

    Article  Google Scholar 

  14. Ferreira VS, Zanoni MVB, Fogg AG (1998) Anal Chim Acta 367:255–259. doi:10.1016/S0003-2670(98)00163-9

    Article  CAS  Google Scholar 

  15. Misztal G (1998) Pharmazie 53:723–724

    CAS  Google Scholar 

  16. Shinde VM, Shabadi CV (1998) Indian J Pharm Sci 60:313–315

    CAS  Google Scholar 

  17. Barnes AR (1995) J Liq Chromatogr 18:3117–3128. doi:10.1080/10826079508010437

    Article  CAS  Google Scholar 

  18. Robbitt JM (1963) Thin-layer chromatography. Chapman and Hall, London

    Google Scholar 

  19. Qureshi SZ, Jamhour RMAQ, Rahman N (1996) J Planar Chromatogr 9:466–469

    CAS  Google Scholar 

  20. Kelani K, Bebawy LI, Abdel-Fattah L (1998) J AOAC Int 81:386–393

    CAS  Google Scholar 

  21. Dhanesar SC (1998) J Planar Chromatogr 11:195–200

    CAS  Google Scholar 

  22. Dhanesar SC (1999) J Planar Chromatogr 12:114–119

    CAS  Google Scholar 

  23. Zarapkar SS, Shivalkar SA, Dhanvate AA, Deshpande PM, Kolte SS (1995) Indian Drugs 32:232–235

    CAS  Google Scholar 

  24. Gupta MM, Verma RK (1996) Indian J Pharm Sci 58:161–162

    CAS  Google Scholar 

  25. Szabó B, Lakatos A, Kõszegi T, Kátay G, Botz L (2005) J AOAC Int 88:1571–1577

    Google Scholar 

  26. Tyrpień K, Bodzek P, Mańka G (2001) Biomed Chromatogr 15:50–55. doi:10.1002/bmc.36

    Article  Google Scholar 

  27. 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

  28. International Conference on Harmonization (2005) Topic Q2 (R1): validation of analytical procedures: text and methodology. http://www.ich.org/LOB/media/MEDIA417.pdf

  29. Pedersen O (2006) Pharmaceutical chemical analysis: methods for identification and limit tests. CRC Press, Taylor and Francis, New York, pp 16–17

    Google Scholar 

  30. 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

    Article  Google Scholar 

  31. 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

  32. Saleh GA, Askal H, Darwish I, El-Shorbagi A (2003) Anal Sci 19:281–287. doi:10.2116/analsci.19.281

    Article  CAS  Google Scholar 

  33. Rodriguez LC, Gracia LG, Loèpez EMA, Sendra JMB (2001) Trends Analyt Chem 20:620–636. doi:10.1016/S0165-9936(01)00111-X

    Article  Google Scholar 

  34. Harvey D (2000) Modern analytical chemistry. McGraw–Hill, Boston, MA, pp 108 and 622

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Azza H. Rageh.

Rights and permissions

Reprints and permissions

About this article

Cite this article

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

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1365/s10337-008-0714-3

Keywords

Navigation