Skip to main content
SpringerLink
Log in

In-line solid-phase extraction–capillary electrophoresis coupled with mass spectrometry for determination of drugs of abuse in human urine

  • Original Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

In-line solid-phase extraction–capillary electrophoresis coupled with mass spectrometric detection (SPE–CE–MS) has been used for determination of 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), codeine (COD), hydrocodeine (HCOD), and 6-acetylmorphine (6AM) in urine. The preconcentration system consists of a small capillary filled with Oasis HLB sorbent and inserted into the inlet section of the electrophoresis capillary. The SPE–CE–MS experimental conditions were optimized as follows: the sample (adjusted to pH 6.0) was loaded at 930 mbar for 60 min, elution was performed with methanol at 50 mbar for 35 s, 60 mmol L−1 ammonium acetate at pH 3.8 was used as running buffer, the separation voltage was 30 kV, and the sheath liquid at a flow rate of 5.0 μL min−1 was isopropanol–water 50:50 (v/v) containing 0.5% acetic acid. Analysis of urine samples spiked with the four drugs and diluted 1:1 (v/v) was studied in the linear range 0.08–10 ng mL−1. Detection limits (LODs) (S/N = 3) were between 0.013 and 0.210 ng mL−1. Repeatability (expressed as relative standard deviation) was below 7.2%. The method developed enables simple and effective determination of these drugs of abuse in urine samples at the levels encountered in toxicology and doping.

Schematic diagram of In-line SPE-CE device

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
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

Abbreviations

6AM:

6-Acetylmorphine

BGE:

Background electrolyte

CE:

Capillary electrophoresis

COD:

Codeine

EDDP:

2-Ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine

HCOD:

Hydrocodeine

ID:

Inner diameter

MS:

Mass spectrometry

SPE:

Solid-phase extraction

References

  1. Gheorghe A, Van Nuijs ALN, Pecceu B, Bervoets L, Jorens PG, Blust R, Neels H, Covaci A (2008) Anal Bioanal Chem 391:1309–1319

    Article  CAS  Google Scholar 

  2. Chiuminatto U, Gosetti F, Dossetto P, Mazzucco E, Zampieri D, Robotti E, Gennaro MC, Marengo E (2010) Anal Chem 82:5636–5645

    Article  CAS  Google Scholar 

  3. Samadinou VF, Anastasiadou K, Papadoyannis IN (2006) J Liq Chromatogr Related Technol 29:889–902

    Article  Google Scholar 

  4. González-Mariño I, Benito J, Rodríguez I, Cela R (2010) J Chromatogr A 1217:1748–1760

    Article  Google Scholar 

  5. Breadmore MC, Dawod M, Quirino JP (2011) Electrophoresis 32:127–148

    Article  CAS  Google Scholar 

  6. Alnajjar A, Idris AM, Multzenberg M, McCord B (2007) J Chromatogr B 856:62–67

    Article  CAS  Google Scholar 

  7. da Costa JL, Tonin FG, Zanolli LA, Chasin AAD, Tavares MFM (2009) Electrophoresis 30(12):2238–2244

    Article  Google Scholar 

  8. Wei F, Zhang M, Feng Y-Q (2006) Electrophoresis 27:1939–1948

    Article  CAS  Google Scholar 

  9. Gottardo R, Polettini A, Sorio D, Pascali JP, Bortolotti F, Liotta E, Tagliaro F (2008) Electrophoresis 29:4078–4087

    Article  CAS  Google Scholar 

  10. Hernández E, Benavente F, Sanz-Nebot V, Barbosa J (2007) Electrophoresis 28:3957–3965

    Article  Google Scholar 

  11. Tagliaro F, Pascali J, Fanigliulo A, Bortolotti F (2010) Electrophoresis 31(1):251–259

    Article  CAS  Google Scholar 

  12. Benavente F, Vescina MC, Hernández E, Sanz-Nebot V, Barbosa J, Guzman NA (2007) J Chromatogr A 1140:205–212

    Article  CAS  Google Scholar 

  13. Almeda S, Arce L, Valcárcel M (2010) Current Anal Chem 6:126–143

    Article  CAS  Google Scholar 

  14. Malá Z, Krivánková L, Gebauer P, Bocek P (2007) Electrophoresis 28:243–253

    Article  Google Scholar 

  15. Saavedra L, Maeso N, Cifuentes A, Barbas C (2007) J Pharm Biomed Anal 44:471–476

    Article  CAS  Google Scholar 

  16. Ramautar R, Somsen GW, de Jong GJ (2010) Electrophoresis 31:44–54

    Article  CAS  Google Scholar 

  17. Puig P, Borrull F, Calull M, Aguilar C (2008) Anal Chim Acta 616:1–8

    Article  CAS  Google Scholar 

  18. Lara FJ, García-Campaña AM, Neusüss C, Alés-Barrero F (2009) J Chromatogr A 1216:3372–3379

    Article  CAS  Google Scholar 

  19. Macià A, Borrull F, Calull M, Benavente F, Hernández E, Sanz-Nebot V, Barbosa J, Aguilar C (2008) J Sep Sci 31:872–880

    Article  Google Scholar 

  20. Hernández E, Benavente F, Sanz-Nebot V, Barbosa J (2008) Electrophoresis 29:3366–3374

    Article  Google Scholar 

  21. Ruiz-Jiménez J, Mata-Granados JM, Luque de Castro MD (2007) Electrophoresis 28:789–798

    Article  Google Scholar 

  22. Saavedra L, Barbas C (2007) J Biochem Biophys Methods 70:289–297

    Article  CAS  Google Scholar 

  23. Botello I, Borrull F, Aguilar C, Calull M (2012) Electrophoresis 33:528–535

    Article  CAS  Google Scholar 

  24. Aturki Z, D'Orazio G, Rocco A, Bortolotti F, Gottardo R, Tagliaro F, Fanali S (2010) Electrophoresis 31(7):1256–1263

    Article  CAS  Google Scholar 

  25. Shappler J, Guillarme D, Prat J, Veuthey J, Rudaz S (2006) Electrophoresis 27:1537–1546

    Article  Google Scholar 

  26. Van Nuijs ALN, Tarcomnicu I, Bervoets L, Blust R, Jorens PG, Neels H, Covaci A (2009) Anal Bioanal Chem 395:819–828

    Article  Google Scholar 

Download references

Acknowledgment

This study was funded by the General Research Directorate of the Spanish Ministerio de Ciencia e Innovación, project CTQ2011-24179 and by Generalitat de Catalunya, Departament d’Innovació, Universitats i Empreses, project 2009 SGR 223.

Conflict of interest

The authors have declared no conflict of interest.

Author information

Authors and Affiliations

  1. Department of Analytical Chemistry and Organic Chemistry, Faculty of Chemistry, Rovira i Virgili University, Marcel·lí Domingo s/n, 43007, Tarragona, Spain

    Igor Botello, Francesc Borrull, Marta Calull & Carme Aguilar

  2. Division of Biomedical Analysis, Department of Pharmaceutical Sciences, Utrecht University, 3584, TC, Utrecht, The Netherlands

    Govert W. Somsen & Gerhardus J. de Jong

Authors
  1. Igor Botello
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Francesc Borrull
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Marta Calull
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Carme Aguilar
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Govert W. Somsen
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Gerhardus J. de Jong
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Carme Aguilar.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Botello, I., Borrull, F., Calull, M. et al. In-line solid-phase extraction–capillary electrophoresis coupled with mass spectrometry for determination of drugs of abuse in human urine. Anal Bioanal Chem 403, 777–784 (2012). https://doi.org/10.1007/s00216-012-5872-3

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-012-5872-3

Keywords

Search

Navigation