Skip to main content
Log in

Electrospray Ionization-Ion Mobility Spectrometry in the Negative Mode Combined with Hollow Fiber Liquid–Liquid–Liquid Microextraction for the Determination of Diclofenac in Urine and Plasma Samples

  • Original
  • Published:
Chromatographia Aims and scope Submit manuscript

Abstract

The combination of hollow fiber liquid–liquid–liquid microextraction and electrospray ionization-ion mobility spectrometry (ESI-IMS) was used for the analysis of diclofenac in biological samples. Diclofenac was extracted from an acidic aqueous sample into methanol as an acceptor phase, through n-dodecane impregnated in the hollow fiber pores. The extracted drug was detected with ESI-IMS in the negative mode. Extraction parameters including pH of donor phase, stirring rate, sample ionic strength, temperature and extraction time were studied. The linearity of the method for the determination of diclofenac was in the range of 100–2000 and 60–2000 µg L−1 for plasma and urine, respectively. The detection limit of the method was also 34 and 21 µg L−1 in the plasma and urine, respectively. The applicability of the method for analyzing the analyte in biological samples was investigated. The method was also applied to analysis of urine and plasma of a healthy volunteer after oral administration of diclofenac.

Graphical abstract

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

Similar content being viewed by others

References

  1. Iliescu T, Baia M, Miclaus V (2004) A Raman spectroscopic study of the diclofenac sodium–β-cyclodextrin interaction. Eur J Pharm Sci 22:487–495

    Article  CAS  Google Scholar 

  2. Todd PA, Sorkin EM (1988) Diclofenac sodium a reappraisal of its pharmacodynamic and pharmacokinetic properties, and therapeutic efficacy. Drugs 35:244–285

    Article  CAS  Google Scholar 

  3. Sharma R, Choudhary S, Kishore N (2012) Insights into the binding of the drugs diclofenac sodium and cefotaxime sodium to serum albumin: calorimetry and spectroscopy. Eur J Pharm Sci 46:435–445

    Article  CAS  Google Scholar 

  4. Bhattacharya SS, Banerjee SB, Ghosh AK, Chattopadhyay P, Verma A, Ghosh A (2013) A RP-HPLC method for quantification of diclofenac sodium released from biological macromolecules. Int J Biol Macromolec 58:354–359

    Article  CAS  Google Scholar 

  5. Yilmaz B (2010) GC–MS determination of diclofenac in human plasma. Chromatogeraphia 71:549–551

    Article  CAS  Google Scholar 

  6. Lee HS, Jeong CK, Choi SJ, Kim SB, Lee MH, Ko JI, Sohn DH (2000) Simultaneous determination of aceclofenac and diclofenac in human plasma by narrowbore HPLC using column-switching. J Pharm Biomed Anal 23:775–781

    Article  CAS  Google Scholar 

  7. Arcelloni C, Lanzi R, Pedercini S, Molteni G, Fermo I, Pontiroli A, Paroni R (2001) High-performance liquid chromatographic determination of diclofenac in human plasma after solid-phase extraction. J Chromatogr B 763:195–200

    Article  CAS  Google Scholar 

  8. Zecca L, Ferrario P, Cost P (1991) Determination of diclofenac and its metabolites in plasma and cerebrospinal fluid by high-performance liquid chromatography with electrochemical detection. J Chromatogr Biomed Appl 567:425–432

    Article  CAS  Google Scholar 

  9. Saraji M, Khaje N (2012) Recent advances in liquid microextraction techniques coupled with mass spectrometry for determination of small-molecule drugs in biological samples. Bioanalysis 4:725–739

    Article  CAS  Google Scholar 

  10. Bello-Lopez MA, Ramos-Payan M, Ocana-Gonzalez JA, Fernandes-Torres R, Callejo-Mochon M (2012) Analytical applications of hollow fiber liquid phase microextraction (HF-LPME): a review. Anal Lett 45:804–830

    Article  CAS  Google Scholar 

  11. Psillakis E, Kalogerakis N (2003) Developments in liquid-phase microextraction. Trends Anal Chem 22:565–574

    Article  CAS  Google Scholar 

  12. Saraji M, Khayamian T, Hashemian Z, Najafi Aslipashaki S, Talebi M (2013) Determination of artemisinin in Artemisia species by hollow fiber-based liquid-phase microextraction and electrospray ionization-ion mobility spectrometry. Anal Methods 5:4190–4195

    Article  CAS  Google Scholar 

  13. Mirmahdieh S, Mardihallaj A, Hashemian Z, Razavizadeh J, Ghaziaskar H, Khayamian T (2011) Analysis of testosterone in human urine using molecularly imprinted solid-phase extraction and corona discharge ion mobility spectrometry. J Sep Sci 34:107–112

    Article  CAS  Google Scholar 

  14. Saraji M, Khayamian T, Hashemian Z (2014) Extraction of methocarbamol from human plasma with a polypyrrole/multiwalled carbon nanotubes composite decorated with magnetic nanoparticles as an adsorbent followed by electrospray ionization ion mobility spectrometry detection. J Sep Sci 37:3518–3525

    Article  CAS  Google Scholar 

  15. Saraji M, Khayamian T, Mirmahdieh S, Hajialiakbari Bidgoli HH (2011) Analysis of amantadine in biological fluids using hollow fiber-based liquid–liquid–liquid microextraction followed by corona discharge mobility spectrometry ion. J Chromatogr B 879:3065–3070

    Article  CAS  Google Scholar 

  16. Reyes-Garces N, Gomez-Ríos GA, Souza Silva EA, Pawliszyn J (2013) Coupling needle trap devices with gas chromatography–ion mobility spectrometry detection as a simple approach for on-site quantitative analysis. J Chromatogr A 1300:193–198

    Article  CAS  Google Scholar 

  17. Alizadeh N, Jafari M, Mohammadi A (2009) Headspace-solid-phase microextraction using a dodecylsulfate-doped polypyrrole film coupled to ion mobility spectrometry for analysis methyl tert-butyl ether in water and gasoline. J Hazard Mater 169:861–867

    Article  CAS  Google Scholar 

  18. Márquez-Sillero I, Aguilera-Herrador E, Cárdenas S, Valcárcel M (2011) Determination of 2,4,6-tricholoroanisole in water and wine samples by ionic liquid-based single-drop microextraction and ion mobility spectrometry. Anal Chim Acta 702:199–204

    Article  Google Scholar 

  19. Lokhnauth JK, Snow NH (2006) Stir-bar sorptive extraction and thermal desorption-ion mobility spectrometry for the determination of trinitrotoluene and l,3,5-trinitro-l,3,5-triazine in water samples. J Chromatogr A 1105:33–38

    Article  CAS  Google Scholar 

  20. Khayamian T, Jafari MT (2007) Design for electrospray ionization-ion mobility spectrometry. Anal Chem 79:3199–3205

    Article  CAS  Google Scholar 

  21. Dwivedi P, Matz LM, Atkinson DA, Hill HH Jr (2004) Electrospray ionization-ion mobility spectrometry: a rapid analytical method for aqueous nitrate and nitrite analysis. Analyst 129:139–144

    Article  CAS  Google Scholar 

  22. Nagaraju D, Huang SD (2007) Determination of triazine herbicides in aqueous samples by dispersive liquid–liquid microextraction with gas chromatography–ion trap mass spectrometry. J Chromatogr A 1161:89–97

    Article  CAS  Google Scholar 

  23. Melwanki MB, Chen WS, Bai HY, Lin TY, Fuh MR (2009) Determination of 7-aminoflunitrazepam in urine by dispersive liquid–liquid microextraction with liquid chromatography–electrospray-tandem mass spectrometry. Talanta 78:618–622

    Article  CAS  Google Scholar 

  24. Xia L, Hu B, Wu Y (2007) Hollow fiber-based liquid–liquid–liquid microextraction combined with high-performance liquid chromatography for the speciation of organomercury. J Chromatogr A 1173:44–51

    Article  CAS  Google Scholar 

  25. Payan MR, Lopez MAB, Fernandez-Torres R, Bernal JLP, Mochon MC (2009) HPLC determination of ibuprofen, diclofenac and salicylic acid using hollow fiber-based liquid phase microextraction (HF-LPME). Anal Chim Acta 653:184–190

    Article  CAS  Google Scholar 

  26. Shukri DSM, Sanagi MM, Ibrahim WAW, Abidin NNZ, Aboul-Enein HY (2015) Liquid chromatographic determination of NSAIDs in urine after dispersive liquid–liquid microextraction based on solidification of floating organic droplets. Chromatographia 78:987–994

    Article  CAS  Google Scholar 

  27. Vazquez AG, Borrull F, Calull M, Aguilar C (2016) Single-drop microextraction combined in-line with capillary electrophoresis for the determination of nonsteroidal anti-inflammatory drugs in urine samples. Electrophoresis 37:274–281

    Article  Google Scholar 

  28. Fotouhi L, Seidi S, Shahsavari F (2016) Optimization of temperature-controlled ionic liquid homogenous liquid phase microextraction followed by high performance liquid chromatography for analysis of diclofenac and mefenamic acid in urine sample. J Iran Chem Soc 13:1289–1299

    Article  CAS  Google Scholar 

  29. Fotouhi L, Seidi S, Yamini Y, Hosseini E (2015) Evaluation of pulsed electromembrane extraction for the analysis of diclofenac and mefenamic acid in biological fluids. Anal Methods 7:2848–2854

    Article  CAS  Google Scholar 

  30. Jin W, Zhang J (2000) Determination of diclofenac sodium by capillary zone electrophoresis with electrochemical detection. J Chromatogr A 868:101–107

    Article  CAS  Google Scholar 

  31. Magiera S, Gulmez S, Michalik A, Baranowska I (2013) Application of statistical experimental design to the optimization of microextraction by packed sorbent for the analysis of nonsteroidal anti-inflammatory drugs in human urine by ultra-high pressure liquid chromatography. J Chromatogr A 1304:1–9

    Article  CAS  Google Scholar 

  32. Sarfraz A, Sarfraz M, Ahmad M (2011) Development and validation of a bioanalytical method for direct extraction of diclofenac potassium form spiked plasma. Trop J Pharm Res 10:663–669

    CAS  Google Scholar 

  33. Kole PL, Millership J, McElnay JC (2011) Determination of diclofenac from paediatric urine samples by stir sorptive extraction (SBSE)–HPLC–UV technique bar. Talanta 85:1948–1958

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors would like to extend their thanks for financial support of this work by the Research Council of Isfahan University of Technology and the Center of Excellence in Chemistry at Isfahan University of Technology.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Mohammad Saraji.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

This study was approved by the local ethics committee of Isfahan University of Technology. The volunteer gave its signed informed consent to participate in the study.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Saraji, M., Maleki, B., Khayamian, T. et al. Electrospray Ionization-Ion Mobility Spectrometry in the Negative Mode Combined with Hollow Fiber Liquid–Liquid–Liquid Microextraction for the Determination of Diclofenac in Urine and Plasma Samples. Chromatographia 80, 951–959 (2017). https://doi.org/10.1007/s10337-017-3292-4

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10337-017-3292-4

Keywords

Navigation