Analytical and Bioanalytical Chemistry

, Volume 400, Issue 2, pp 527–534 | Cite as

Simultaneous determination of weakly ionizable analytes in urine and plasma samples by transient pseudo-isotachophoresis in capillary zone electrophoresis

  • Igor Botello
  • Francesc Borrull
  • Marta Calull
  • Carme AguilarEmail author
Original Paper


A rapid method for the simultaneous determination of several non-steroidal anti-inflammatory drugs (NSAIDs) in human plasma and urine was developed using transient pseudo-isotachophoresis (ITP) in capillary zone electrophoresis (CZE). The influence of different parameters on resolution and preconcentration efficiency, such as background electrolyte (BGE) composition, sample injection, sample matrix composition, and pH, were studied to optimize the transient pseudo-ITP performance. Optimized conditions were a BGE consisting of 100 mM Na2B4O7 in 10% aqueous MeOH solution and hydrodynamic injection of the sample at 50 mbar for 90 s. The sample was prepared in a solution mixture of 1% NaCl/ethanol (30:70 v/v) at pH 10. Our results show that this simple strategy offers improved sensitivity compared to conventional CZE analysis, reaching a 45-fold preconcentration factor. The detection limits (LODs) were as low as 0.07 mg/L for standard samples with good repeatability (values of relative standard deviation, %RSD < 11%). The method was applied to the analysis of NSAIDs in biological samples. Validation for human plasma and urine samples demonstrated good linearity, low detection limits, and satisfactory repeatability values.


Capillary electrophoresis Non-steroidal anti-inflammatory drugs Plasma samples Transient pseudo-isotachophoresis Urine samples 



background electrolyte


capillary electrophoresis


capillary zone electrophoresis




non-steroidal anti-inflammatory drug


sensitivity enhancement factor

Transient pseudo-ITP

transient pseudo-isotachophoresis



This study was funded by the General Research Directorate of the Spanish Ministry of Science and Technology, projects CTM2008-06847-C02-01/TECNO and CTM2008-0825 and by the Generalitat de Catalunya, Department d’Innovació, Universitats i Empreses, project 2009 SGR 223.


  1. 1.
    Lees P, Landoni MF, Giraudel J, Toutain PL (2004) J Vet Pharmacol Ther 27:479–490CrossRefGoogle Scholar
  2. 2.
    Jager AD, Ellis H, Hundt HKL, Swart KJ, Hundt AF (1999) J Chromatogr B 729:183–189CrossRefGoogle Scholar
  3. 3.
    Navas N, Ureña R, Capitan-Vallvey L-F (2008) Chromatographia 67:55–61CrossRefGoogle Scholar
  4. 4.
    Hundal O, Kvien TK, Glennas A, Andrup O, Karstenson B, Theon JE, Rugstad HE, Scand (1993) J Rheumatol 22:183–189Google Scholar
  5. 5.
    Huang YJ, Wang GR, Huang KP, Hsieh YF, Liu CY (2009) Electrophoresis 30:3964–3970CrossRefGoogle Scholar
  6. 6.
    Macià A, Borrull F, Calull M, Aguilar C (2007) Trends Anal Chem 26:133–153CrossRefGoogle Scholar
  7. 7.
    Dawod M, Breadmore MC, Guijt RM, Haddad PR (2008) J Chromatogr A 1189:278–284CrossRefGoogle Scholar
  8. 8.
    Dawod M, Breadmore MC, Guijt RM, Haddad PR (2009) J Chromatogr A 1216:3380–3386CrossRefGoogle Scholar
  9. 9.
    Kuo YL, Liu WL, Hsieh SH, Huang HY (2010) Anal Sci 26:703–707CrossRefGoogle Scholar
  10. 10.
    Gentili A (2007) Anal Bioanal Chem 387:1185–1202CrossRefGoogle Scholar
  11. 11.
    Botello I, Borrull F, Calull M, Aguilar C (2010) Electrophoresis 31:2964–2973CrossRefGoogle Scholar
  12. 12.
    Macià A, Borrull F, Aguilar C, Calull M (2003) Electrophoresis 24:2779–2787CrossRefGoogle Scholar
  13. 13.
    Macià A, Borrull F, Calull M, Aguilar C (2005) Electrophoresis 26:970–979CrossRefGoogle Scholar
  14. 14.
    Macià A, Borrull F, Calull M, Aguilar C (2006) J Chromatogr A 1117:234–245CrossRefGoogle Scholar
  15. 15.
    Suntornsuk L (2010) Anal Bioanal Chem 398:29–52CrossRefGoogle Scholar
  16. 16.
    Shihabi ZK (1998) J Chromatogr A 817:25–30CrossRefGoogle Scholar
  17. 17.
    Friedberg M, Hinsdale M, Shihabi ZK (1997) J Chromatogr A 781:35–42CrossRefGoogle Scholar
  18. 18.
    Shihabi ZK (2009) Electrophoresis 30:1516–1521CrossRefGoogle Scholar
  19. 19.
    Shihabi ZK (2002) Electrophoresis 23:1612–1617CrossRefGoogle Scholar
  20. 20.
    Pai Y-F, Lin C-C, Liu C-Y (2004) Electrophoresis 25:569–577CrossRefGoogle Scholar
  21. 21.
    Kong Y, Zheng N, Zhang Z, Gao R (2003) J Chromatogr B 795:9–15CrossRefGoogle Scholar
  22. 22.
    Kong Y (2006) J Liq Chromatogr Relat Technol 29:1561–1573CrossRefGoogle Scholar
  23. 23.
    Kubalczyk P, Bald E (2006) Anal Bioanal Chem 384:1181–1185CrossRefGoogle Scholar
  24. 24.
    Friedberg M, Shihabi ZK (1997) J Chromatogr B 695:193–198CrossRefGoogle Scholar
  25. 25.
    Lu C, Jong Y, Ferrance J, Ko W, Wu S (2007) Electrophoresis 28:3290–3295CrossRefGoogle Scholar
  26. 26.
    Khurana TK, Santiago JG (2008) Anal Chem 80:6300–6309CrossRefGoogle Scholar
  27. 27.
    Veraart JR, Groot MCE, Gooijer C, Lingeman H, Velthorst NH, Brinkman UAT (1999) Analyst 124:115–118CrossRefGoogle Scholar

Copyright information

© Springer-Verlag 2011

Authors and Affiliations

  • Igor Botello
    • 1
  • Francesc Borrull
    • 1
  • Marta Calull
    • 1
  • Carme Aguilar
    • 1
    Email author
  1. 1.Departament de Química Analítica i Química Orgànica, Facultat de QuímicaUniversitat Rovira i VirgiliTarragonaSpain

Personalised recommendations