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Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry.
Anal Chim Acta. 2015 Jul 02; 882:112-26.AC

Abstract

This is the first study presenting a multi-residue method allowing for comprehensive analysis of several chiral pharmacologically active compounds (cPACs) including beta-blockers, antidepressants and amphetamines in wastewater and digested sludge at the enantiomeric level. Analysis of both the liquid and solid matrices within wastewater treatment is crucial to being able to carry out mass balance within these systems. The method developed comprises filtration, microwave assisted extraction and solid phase extraction followed by chiral liquid chromatography coupled with tandem mass spectrometry to analyse the enantiomers of 18 compounds within all three matrices. The method was successfully validated for 10 compounds within all three matrices (amphetamine, methamphetamine, MDMA, MDA, venlafaxine, desmethylvenlafaxine, citalopram, metoprolol, propranolol and sotalol), 7 compounds validated for the liquid matrices only (mirtazapine, salbutamol, fluoxetine, desmethylcitalopram, atenolol, ephedrine and pseudoephedrine) and 1 compound (alprenolol) passing the criteria for solid samples only. The method was then applied to wastewater samples; cPACs were found at concentration ranges in liquid matrices of: 1.7 ng L(-1) (metoprolol) - 1321 ng L(-1) (tramadol) in influent, <LOD (desmethylcitalopram and metoprolol) - 506 ng L(-1) in effluent, and in solid matrix digested sludge: 0.4 ng g(-1) (metoprolol) - 275 ng g(-1) (citalopram). Enantiomeric profiling revealed that studied compounds were present in analysed samples in non-racemic composition. Furthermore, enantiomeric composition of studied analytes differed in liquid and solid matrices. This demonstrates that not analysing the solid fraction of wastewater may lead to over-estimation of the removal rates of cPACs as well as possible misrepresentation of the enantiomeric fraction of the compounds as they leave the wastewater treatment plant. Consequently risks from cPACs entering the environment might be higher than anticipated.

Authors+Show Affiliations

University of Bath, Department of Chemistry, Faculty of Science, Bath BA2 7AY, UK.University of Bath, Department of Chemistry, Faculty of Science, Bath BA2 7AY, UK.University of Bath, Department of Chemistry, Faculty of Science, Bath BA2 7AY, UK.University of Bath, Department of Chemistry, Faculty of Science, Bath BA2 7AY, UK. Electronic address: b.kasprzyk-hordern@bath.ac.uk.

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

26043098

Citation

Evans, Sian E., et al. "Determination of Chiral Pharmaceuticals and Illicit Drugs in Wastewater and Sludge Using Microwave Assisted Extraction, Solid-phase Extraction and Chiral Liquid Chromatography Coupled With Tandem Mass Spectrometry." Analytica Chimica Acta, vol. 882, 2015, pp. 112-26.
Evans SE, Davies P, Lubben A, et al. Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry. Anal Chim Acta. 2015;882:112-26.
Evans, S. E., Davies, P., Lubben, A., & Kasprzyk-Hordern, B. (2015). Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry. Analytica Chimica Acta, 882, 112-26. https://doi.org/10.1016/j.aca.2015.03.039
Evans SE, et al. Determination of Chiral Pharmaceuticals and Illicit Drugs in Wastewater and Sludge Using Microwave Assisted Extraction, Solid-phase Extraction and Chiral Liquid Chromatography Coupled With Tandem Mass Spectrometry. Anal Chim Acta. 2015 Jul 2;882:112-26. PubMed PMID: 26043098.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry. AU - Evans,Sian E, AU - Davies,Paul, AU - Lubben,Anneke, AU - Kasprzyk-Hordern,Barbara, Y1 - 2015/03/28/ PY - 2014/11/01/received PY - 2015/03/14/revised PY - 2015/03/24/accepted PY - 2015/6/5/entrez PY - 2015/6/5/pubmed PY - 2016/3/2/medline KW - Chiral chromatography coupled with mass spectrometry KW - Chiral drugs KW - Illicit KW - Pharmaceuticals KW - Sludge KW - Wastewater SP - 112 EP - 26 JF - Analytica chimica acta JO - Anal Chim Acta VL - 882 N2 - This is the first study presenting a multi-residue method allowing for comprehensive analysis of several chiral pharmacologically active compounds (cPACs) including beta-blockers, antidepressants and amphetamines in wastewater and digested sludge at the enantiomeric level. Analysis of both the liquid and solid matrices within wastewater treatment is crucial to being able to carry out mass balance within these systems. The method developed comprises filtration, microwave assisted extraction and solid phase extraction followed by chiral liquid chromatography coupled with tandem mass spectrometry to analyse the enantiomers of 18 compounds within all three matrices. The method was successfully validated for 10 compounds within all three matrices (amphetamine, methamphetamine, MDMA, MDA, venlafaxine, desmethylvenlafaxine, citalopram, metoprolol, propranolol and sotalol), 7 compounds validated for the liquid matrices only (mirtazapine, salbutamol, fluoxetine, desmethylcitalopram, atenolol, ephedrine and pseudoephedrine) and 1 compound (alprenolol) passing the criteria for solid samples only. The method was then applied to wastewater samples; cPACs were found at concentration ranges in liquid matrices of: 1.7 ng L(-1) (metoprolol) - 1321 ng L(-1) (tramadol) in influent, <LOD (desmethylcitalopram and metoprolol) - 506 ng L(-1) in effluent, and in solid matrix digested sludge: 0.4 ng g(-1) (metoprolol) - 275 ng g(-1) (citalopram). Enantiomeric profiling revealed that studied compounds were present in analysed samples in non-racemic composition. Furthermore, enantiomeric composition of studied analytes differed in liquid and solid matrices. This demonstrates that not analysing the solid fraction of wastewater may lead to over-estimation of the removal rates of cPACs as well as possible misrepresentation of the enantiomeric fraction of the compounds as they leave the wastewater treatment plant. Consequently risks from cPACs entering the environment might be higher than anticipated. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/26043098/Determination_of_chiral_pharmaceuticals_and_illicit_drugs_in_wastewater_and_sludge_using_microwave_assisted_extraction_solid_phase_extraction_and_chiral_liquid_chromatography_coupled_with_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0003-2670(15)00415-8 DB - PRIME DP - Unbound Medicine ER -