SpringerLink
Log in

Quantification of drugs of abuse in municipal wastewater via SPE and direct injection liquid chromatography mass spectrometry

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

Abstract

We present an isotopic-dilution direct injection reversed-phase liquid chromatography–tandem mass spectrometry method for the simultaneous determination of 23 drugs of abuse, drug metabolites, and human-use markers in municipal wastewater. The method places particular emphasis on cocaine; it includes 11 of its metabolites to facilitate assessment of routes of administration and to enhance the accuracy of estimates of cocaine consumption. Four opioids (6-acetylmorphine, morphine, hydrocodone, and oxycodone) are also included, along with five phenylamine drugs (amphetamine, methamphetamine, 3,4-methylenedioxy-methamphetamine, methylbenzodioxolyl-butanamine, and 3,4-methylenedioxy-N-ethylamphetamine) and two human-use markers (cotinine and creatinine). The method is sufficiently sensitive to directly quantify (without preconcentration) 18 analytes in wastewater at concentrations less than 50 ng/L. We also present a modified version of this method that incorporates solid-phase extraction to further enhance sensitivity. The method includes a confirmatory LC separation (selected by evaluating 13 unique chromatographic phases) that has been evaluated using National Institute of Standards and Technology Standard Reference Material 1511 Multi-Drugs of Abuse in Freeze-Dried Urine. Seven analytes (ecgonine methyl ester, ecgonine ethyl ester, anhydroecgonine methyl ester, m-hydroxybenzoylecgonine, p-hydroxybenzoyl-ecgonine, ecgonine, and anhydroecgonine) were detected for the first time in a wastewater sample.

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

Access this article

Log in via an institution

Subscribe and save

Springer+ Basic
EUR 32.99 /Month
  • Get 10 units per month
  • Download Article/Chapter or Ebook
  • 1 Unit = 1 Article or 1 Chapter
  • Cancel anytime
Subscribe now

Buy Now

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

Similar content being viewed by others

References

  1. Daughton CG, Jones-Lepp TL (2001) Pharmaceuticals and personal care products in the environment. ACS Symp Ser 791:348–364

    Article  CAS  Google Scholar 

  2. Jones-Lepp TL, Alvarez DA, Petty JD, Huckins JN (2004) Arch Environ Contam Toxicol 47:427–439

    Article  CAS  Google Scholar 

  3. Castiglioni S, Zuccato E, Crisci E, Chiabrando C, Fanelli R, Bagnati R (2006) Anal Chem 78:8421–8429

    Article  CAS  Google Scholar 

  4. Hummel D, Loffler D, Fink G, Ternes TA (2006) Environ Sci Technol 40:7321–7328

    Article  CAS  Google Scholar 

  5. Boleda MR, Galceran MT, Ventura FJ (2007) Chromatogr A 1175:38–48

    Article  CAS  Google Scholar 

  6. Bones J, Thomas KV, Paull BJ (2007) Environ Monit 9:701–707

    Article  CAS  Google Scholar 

  7. Huerta-Fontela M, Galceran MT, Ventura F (2007) Anal Chem 79:3821–3829

    Article  CAS  Google Scholar 

  8. Kasprzyk-Hordem B, Dinsdale RM, Guwy AJ (2007) J Chromatogr A 1161:132–145

    Article  Google Scholar 

  9. Chiaia AC, Banta-Green C, Field J (2008) Environ Sci Technol 42:8841–8848

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

  11. Postigo C, de Ada MJL, Barcelo D (2008) Trac-Trends Anal Chem 27:1053–1069

    Article  CAS  Google Scholar 

  12. Postigo C, de Alda MJL, Barcelo D (2008) Anal Chem 80:3123–3134

    Article  CAS  Google Scholar 

  13. Bijlsma L, Sancho JV, Pitarch E, Ibanez M, Hernandez F (2009) J Chromatogr A 1216:3078–3089

    Article  CAS  Google Scholar 

  14. Mari F, Politi L, Biggeri A, Accetta G, Trignano C, Di Padua M, Bertol E (2009) Forensic Sci Int 189:88–92

    Article  CAS  Google Scholar 

  15. van Nuijs ALN, Pecceu B, Theunis L, Dubois N, Charlier C, Jorens PG, Bervoets L, Blust R, Neels H, Covaci A (2009) Environ Pollut 157:123–129

    Article  Google Scholar 

  16. Cook CE, Jeffcoat AR (1984) Pharmacokinetics and pharmacodynamics of psychoactive drugs. Biomedical, Foster City, pp 48–74

    Google Scholar 

  17. Jatlow P (1988) Yale J Biol Med 61:105–113

    CAS  Google Scholar 

  18. Baselt RC (2004) Disposition of toxic drugs and chemicals in man. Biomedical, Foster City

    Google Scholar 

  19. Paul BD, Lalani S, Bosy T, Jacobs AJ, Huestis MA (2005) Biomed Chromatogr 19:677–688

    Article  CAS  Google Scholar 

  20. Jacob P, Lewis ER, Eliasbaker BA, Jones RTJ (1990) Anal Toxicol 14:353–357

    CAS  Google Scholar 

  21. Cone EJ, Hillsgrove M, Darwin WD (1994) Clin Chem 40:1299–1305

    CAS  Google Scholar 

  22. McCancekatz EF, Price LH, McDougle CJ, Kosten TR, Black JE, Jatlow PI (1993) Psychopharmacologia 111:39–46

    Article  CAS  Google Scholar 

  23. Zuccato E, Chiabrando C, Castiglioni S, Bagnati R, Fanelli R (2008) Environ Health Perspect 116:1027–1032

    Article  CAS  Google Scholar 

  24. Kasprzyk-Hordern B, Dinsdale RM, Guwy AJ (2009) Environ Pollut 157:1773–1777

    Article  CAS  Google Scholar 

  25. van Nuijs ALN, Pecceu B, Theunis L, Dubois N, Charlier C, Jorens PG, Bervoets L, Blust R, Meulemans H, Neels H, Covaci A (2009) Addiction 104:734–741

    Article  Google Scholar 

  26. van Nuijs ALN, Pecceu B, Theunis L, Dubois N, Charlier C, Jorens PG, Bervoets L, Blust R, Neels H, Covaci A (2009) Water Res 43:1341–1349

    Article  Google Scholar 

  27. Bisceglia KJ (2010) Ph.D. dissertation. Johns Hopkins University, Baltimore

  28. Peck AM, Heltsley RM, Kucklick JR, Lippa KA, Schantz MM (2007) Abstract in SETAC North America 28th Annual Meeting Abstract Book

  29. Kraemer T, Paul LD (2007) Anal Bioanal Chem 388:1415–1435

    Article  CAS  Google Scholar 

  30. Pizzolato TM, de Alda MJL, Barcelo D (2007) Trac-Trends Anal Chem 26:609–624

    Article  CAS  Google Scholar 

  31. Johansen SS, Bhatia HM (2007) J Chromatogr B 852:338–344

    Article  CAS  Google Scholar 

  32. Jagerdeo E, Montgomery MA, LeBeau MA, Sibum M (2008) J Chromatogr B 874:15–20

    Article  CAS  Google Scholar 

  33. Benijts T, Dams R, Lambert W, De Leenheer A (2004) J Chromatogr A 1029:153–159

    Article  CAS  Google Scholar 

  34. Giroud C, Michaud K, Sporkert F, Eap C, Augsburger M, Cardinal P, Mangin P (2004) J Anal Toxicol 28:464–474

    CAS  Google Scholar 

  35. Bisceglia KJ, Roberts AL, Lippa KA (2010) Environ Sci Tech

  36. ASTM International (2008) ASTM standard D5905-98: standard practice for the preparation of substitute wastewater. ASTM International, West Conshohocken

    Google Scholar 

  37. Hubaux A, Vos G (1970) Anal Chem 42:849

    Article  CAS  Google Scholar 

  38. National Institute of Standards and Technology (2006) Standard reference material 1511: multi-drugs of abuse in freeze-dried urine. National Institute of Standards and Technology, Gaithersburg

    Google Scholar 

  39. Bell DS, Jones AD (2005) J Chromatogr A 1073:99–109

    Article  CAS  Google Scholar 

  40. Snyder LR, Dolan JW (2006) High-performance gradient elution: the practical application of the linear-solvent-strength model. Wiley, New York

    Book  Google Scholar 

  41. Schlichtherle-Cerny H, Affolter M, Cerny C (2003) Anal Chem 75:2349–2354

    Article  CAS  Google Scholar 

  42. Hemstrom P, Irgum K (2006) J Sep Sci 29:1784–1821

    Article  Google Scholar 

  43. Matuszewski BK, Constanzer ML, Chavez-Eng CM (2003) Anal Chem 75:3019–3030

    Article  CAS  Google Scholar 

Download references

Acknowledgements

We wish to thank Aaron Peck and Rebecca Heltsley of NIST for their initial efforts in LC/MS/MS method development. We also thank William Jeffrey (former NIST Director) for bringing this measurement need to our attention.

Conflicts of interest

Certain commercial equipment, instruments, or materials are identified in this paper to specify adequately the experimental procedure. Such identification does not imply recommendation or endorsement by the National Institute of Standards and Technology, nor does it imply that the materials or equipment identified are necessarily the best available for the purpose.

Author information

Author notes

  1. Kevin J. Bisceglia

    Present address: Chemistry Department, Bard High School Early College, 30-20 Thomson Avenue, Queens, NY, 11101, USA

Authors and Affiliations

  1. Department of Geography and Environmental Engineering, Johns Hopkins University, 3400 North Charles Street, Baltimore, MD, 21218, USA

    Kevin J. Bisceglia & A. Lynn Roberts

  2. Analytical Chemistry Division, National Institute of Standards and Technology, 100 Bureau Drive, Stop 8392, Gaithersburg, MD, 20899-8392, USA

    Kevin J. Bisceglia, Michele M. Schantz & Katrice A. Lippa

Authors
  1. Kevin J. Bisceglia
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. A. Lynn Roberts
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Michele M. Schantz
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Katrice A. Lippa
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Katrice A. Lippa.

Electronic supplementary material

Below is the link to the electronic supplementary material.

ESM 1

(DOC 1.23 mb)

Rights and permissions

Reprints and permissions

About this article

Cite this article

Bisceglia, K.J., Roberts, A.L., Schantz, M.M. et al. Quantification of drugs of abuse in municipal wastewater via SPE and direct injection liquid chromatography mass spectrometry. Anal Bioanal Chem 398, 2701–2712 (2010). https://doi.org/10.1007/s00216-010-4191-9

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-010-4191-9

Keywords

Search

Navigation