Skip to main content
SpringerLink
Log in

Determination of Betamethasone and Dexamethasone in Human Urine and Serum by MEKC After an Experimental Design

  • Full Short Communication
  • Published:
Chromatographia Aims and scope Submit manuscript

Abstract

A simple and reliable micellar electrokinetic capillary chromatography method has been presented for the simultaneous determination of betamethasone (BM) and its epimer dexamethasone (DM) in human urine and serum. A three level full factorial experimental design was employed to search for the optimum conditions. Rapid and baseline separation of BM and DM was obtained within 7 min with the optimum conditions of 30 mM borax buffer, 30 mM sodium dodecyl sulfate at pH 10.0, separation voltage at 18 kV, injection time 15 s at a height of 10 cm, using sodium sorbate as internal standard. The proposed method was validated with respect to stability, precision, linearity and accuracy. Good relationship between peak area ratio and analyte concentration was linear over 30–1,000 µg mL−1 for BM and DM with correlation coefficients ≥0.9993. Relative standard deviations of the method were all less than 4.50% in the intra-day and inter-day analysis. The developed method was applied to assay spiked human urine and serum samples containing both compounds with recoveries in the range of 97.5–100.5%.

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

Access this article

Log in via an institution

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

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2

Similar content being viewed by others

References

  1. Litter M (1986) Farmacología experimentaly clínica. El Ateneo, Buenos Aires

    Google Scholar 

  2. Olympic Movement Antidoping Code (2003) International Olympic Committee, Lausanne

  3. Das B, Datta K, Das SK (1985) J Liq Chromatogr Relat Technol 8:3009–3016. doi:10.1080/01483918508076616

    Article  CAS  Google Scholar 

  4. Iglesias Y, Fente C, Vázquez BI, Franco C, Cepeda A, Mayob S (2002) Anal Chim Acta 468:43–52. doi:10.1016/S0003-2670(02)00598-6

    Article  CAS  Google Scholar 

  5. Vázquez BI, Feás X, Lolo M, Fente CA, Franco CM, Cepeda A (2005) Luminescence 20:197–204. doi:10.1002/bio.814

    Article  Google Scholar 

  6. Ku YR, Wen KC, Ho LK, Chang YS (1999) J Food Drug Anal 7:123–130

    CAS  Google Scholar 

  7. Quintana MC, Blanco MH, Lacal J, Hernandez L (2001) J Liq Chromatogr Relat Technol 24:735–745. doi:10.1081/JLC-100103407

    Article  CAS  Google Scholar 

  8. Quintana MC, Ramos L, González MJ, Blanco MH, Hernández L (2004) J Sep Sci 27:53–58. doi:10.1002/jssc.200301569

    Article  CAS  Google Scholar 

  9. Ma Q, Wang C, Wang X, Bai H, Chen W, Wu T et al (2007) Chin J Chromatogr A 25:541–545

    CAS  Google Scholar 

  10. Amendola L, Garribba F, Botrè F (2003) Anal Chim Acta 489:233–243. doi:10.1016/S0003-2670(03)00703-7

    Article  CAS  Google Scholar 

  11. Fiori M, Pierdominici E, Longo F, Brambilla G (1998) J Chromatogr A 807:219–227. doi:10.1016/S0021-9673(98)00072-7

    Article  CAS  Google Scholar 

  12. Van den Hauwe O, Castro Perez J, Claereboudt J, Van Peteghem C (2001) Rapid Commun Mass Spectrom 15:857–861

    Article  Google Scholar 

  13. Van den Hauwea O, Dumoulin F, Antignac JP, Bouche MP, Elliott C, Van Peteghema C (2002) Anal Chim Acta 473:127–134

    Article  Google Scholar 

  14. Draisci R, Marchiafava C, Palleschi L, Cammarata P, Cavallia S (2001) J Chromatogr B Analyt Technol Biomed Life Sci 753:217–223. doi:10.1016/S0378-4347(00)00544-2

    Article  CAS  Google Scholar 

  15. Noben JP, Gielen B, Royackers E, Missotten M, Jacobs A, Raus J (2002) J Rapid Commun Mass Spectrom 16:1590–1594

    Article  CAS  Google Scholar 

  16. Antignac JP, Le Bizec B, Monteau F, Andre F (2002) J Mass Spectrom 37:69–75. doi:10.1002/jms.260

    Article  CAS  Google Scholar 

  17. Sangiorgi E, Curatolo M, Assini W, Bozzoni E (2003) Anal Chim Acta 483:259–267. doi:10.1016/S0003-2670(02)01534-9

    Article  CAS  Google Scholar 

  18. Baiocchi C, Brussino M, Pazzi M, Medana C, Marini C, Genta E (2003) Chromatographia 58:11–14

    CAS  Google Scholar 

  19. Deventer K, Delbeke FT (2003) Rapid Commun Mass Spectrom 17:2107–2114. doi:10.1002/rcm.1157

    Article  CAS  Google Scholar 

  20. Arthur KE, Wolff JC, Carrier DJ (2004) Rapid Commun Mass Spectrom 18:678–684. doi:10.1002/rcm.1386

    Article  CAS  Google Scholar 

  21. Taylor RL, Grebe SK, Singh RJ (2004) Clin Chem 50:2345–2352. doi:10.1373/clinchem.2004.033605

    Article  CAS  Google Scholar 

  22. Luo Y, Uboh CE, Soma LR, Guan FY, Rudy JA, Tsang DS (2005) Rapid Commun Mass Spectrom 19:825–832. doi:10.1002/rcm.1851

    Article  CAS  Google Scholar 

  23. Luo Y, Uboh CE, Soma LR, Guan FY, Rudy JA, Tsang DS (2005) Rapid Commun Mass Spectrom 19:1245–1256. doi:10.1002/rcm.1916

    Article  CAS  Google Scholar 

  24. Toube ME, van Engelen MC, Georgakopoulus C, van Rhijn JA, Nielen MWF (2007) Anal Chim Acta 586:137–146. doi:10.1016/j.aca.2006.09.058

    Article  Google Scholar 

  25. McDonalda M, Granelli K, Sjöberg P (2007) Anal Chim Acta 588:20–25. doi:10.1016/j.aca.2007.01.075

    Article  Google Scholar 

  26. Peña-García-Brioles D, Gonzalo-Lumbreras R, Izquierdo-Hornillos R, Santos-Montes A (2004) J Pharm Biomed Anal 36:65–71. doi:10.1016/j.jpba.2004.05.007

    Article  Google Scholar 

  27. De Wasch K, De Brabander HF, Van de Wiele M, Vercammen J, Courtheyn D, Impens S (2001) J Chromatogr A 926:79–86. doi:10.1016/S0021-9673(01)00744-0

    Article  Google Scholar 

  28. Pujos E, Flament-Waton MM, Paisse O, Grenier-Loustalot MF (2005) Anal Bioanal Chem 381:244–254. doi:10.1007/s00216-004-2890-9

    Article  CAS  Google Scholar 

  29. Taylor MR, Teale P (1997) J Chromatogr A 768:89–95. doi:10.1016/S0021-9673(96)00942-9

    Article  CAS  Google Scholar 

  30. Spikmans V, Lane SJ, Smith NW (2000) Chromatographia 51:18–24. doi:10.1007/BF02490690

    Article  CAS  Google Scholar 

  31. Lucangioli SE, Rodríguez VG, Fernández Otero GC, Vizioli NM, Carducci CN (1997) J Capillary Electrophor 4:27–31

    CAS  Google Scholar 

  32. Lin M, Wu N (1999) J Pharm Biomed Anal 19:945–954. doi:10.1016/S0731-7085(98)00288-X

    Article  CAS  Google Scholar 

  33. Huang WL, Harper CG, Evans SF, Newnham JP, Dunlop SA (2001) Int J Dev Neurosci 19:487–493. doi:10.1016/S0736-5748(01)00035-1

    Article  CAS  Google Scholar 

  34. Lucangioli SE, Carducci CN, Scioscia SL, Carlucci A, Bregni C, Kenndler E (2003) Electrophoresis 24:984–991. doi:10.1002/elps.200390142

    Article  CAS  Google Scholar 

  35. Kuo CY, Wu SM (2005) J Sep Sci 28:144–148. doi:10.1002/jssc.200401905

    Article  CAS  Google Scholar 

  36. Baeyens V, Varesio E, Veuthey JL, Gurny R (1997) J Chromatogr B Analyt Technol Biomed Life Sci 692:222–226. doi:10.1016/S0378-4347(96)00494-X

    Article  Google Scholar 

  37. Raith K, Althoff E, Banse J, Neidhardt H, Neubert RH (1998) Electrophoresis 19:16–17. doi:10.1002/elps.1150191618

    Article  Google Scholar 

  38. Gallego JML, Arroyo JP (2001) J Anal Chem 370:973–975. doi:10.1007/s002160100895

    Article  Google Scholar 

  39. Nepote AJ, Vera-Candiotti L, Williner MR, Damiani PC, Olivieri AC (2003) Anal Chim Acta 489:77–84. doi:10.1016/S0003-2670(03)00714-1

    Article  CAS  Google Scholar 

  40. Du B, Wu CL, Zhang ZZ (2005) J Zhengzhou Univ Med Sci 41:154–156

    Google Scholar 

  41. Candioti LV, Robles JC, Mantovani VE, Goicoechea H (2006) Talanta 69:140–147. doi:10.1016/j.talanta.2005.09.021

    Article  CAS  Google Scholar 

  42. Liang GL, Lian Y (2006) West China J Pharm Sci 21:286–287

    CAS  Google Scholar 

  43. Lee RJ, Liu Z, Zou HF, Ni JY, Zhang YK (2000) J Microcolumn Sep 12:356–365. doi :10.1002/1520-667X(2000)12:6<356::AID-MCS4>3.0.CO;2-G

    Article  CAS  Google Scholar 

  44. Loukasa YL, Sabbah S, Scriba GKE (2001) J Chromatogr A 931:141–152. doi:10.1016/S0021-9673(01)01179-7

    Article  Google Scholar 

  45. Capella-Peiro ME, Bossi A, Esteve-Romero J (2006) Anal Biochem 352:41–49. doi:10.1016/j.ab.2005.12.028

    Article  CAS  Google Scholar 

  46. Lin YH, Yang YH, Wu SM (2007) J Pharm Biomed Anal 44:279–282. doi:10.1016/j.jpba.2007.02.004

    Article  CAS  Google Scholar 

  47. IFPMA (ed) (1994) Validation of analytical procedures: test and methodology. ICH harmonised tripartite guideline, Geneva

Download references

Author information

Authors and Affiliations

  1. College of Chemistry, Jilin University, 130022, Changchun, China

    Lihua Song, Jianguo Bai & Weihong Zhou

Authors
  1. Lihua Song
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Jianguo Bai
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Weihong Zhou
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Weihong Zhou.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Song, L., Bai, J. & Zhou, W. Determination of Betamethasone and Dexamethasone in Human Urine and Serum by MEKC After an Experimental Design. Chroma 68, 287–293 (2008). https://doi.org/10.1365/s10337-008-0692-5

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1365/s10337-008-0692-5

Keywords

Search

Navigation