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Screening and selective quantification of illicit drugs in wastewater by mixed-mode solid-phase extraction and quadrupole-time-of-flight liquid chromatography-mass spectrometry.
Anal Chem. 2012 Feb 07; 84(3):1708-17.AC

Abstract

For the first time, a mixed-mode solid-phase extraction with fractionation of basic analytes from neutral and acidic species during cartridge elution and liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) was combined for the quantitative determination of 24 illicit drugs and metabolites in urban sewage samples. The effects of several sample preparation and instrumental parameters in the sensitivity and selectivity of the quantitative method are thoroughly discussed. Under final working conditions, recoveries above 63% and 82% were attained for all species in raw and treated sewage, respectively; whereas, the limits of quantification of the method, defined for a signal-to-noise of 10 (S/N = 10), ranged from 2 to 50 ng L(-1). Sequential elution of mixed-mode cartridges allowed a significant reduction of matrix effects observed during electrospray ionization of basic drugs versus those measured for hydrophilic balance reversed-phase sorbents and the same mixed-mode polymer without fractionated elution. Analysis of raw wastewater samples confirmed the ubiquity of cocaine (COC), benzoylecgonine (BE), and 11-nor-9-carboxy-Δ(9)-tetrahydrocannabinol (THCCOOH) in this matrix. The capability of the above methodology to identify new illicit drugs and/or metabolites in sewage samples is also discussed. With this aim, a two step strategy is proposed. First, high-resolution MS chromatograms, acquired throughout each chromatographic run, are automatically searched against an in-house built database, a reduced list of candidate drugs is generated, and the corresponding extracted ion chromatograms are obtained. In a further LC run, the tandem mass spectrometry (MS/MS) spectra of unknown peaks are acquired using different collision energies and compared with those existing in public libraries, or interpreted, to assign the unknown peak to one of the previously selected candidates.

Authors+Show Affiliations

Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

22185484

Citation

González-Mariño, Iria, et al. "Screening and Selective Quantification of Illicit Drugs in Wastewater By Mixed-mode Solid-phase Extraction and Quadrupole-time-of-flight Liquid Chromatography-mass Spectrometry." Analytical Chemistry, vol. 84, no. 3, 2012, pp. 1708-17.
González-Mariño I, Quintana JB, Rodríguez I, et al. Screening and selective quantification of illicit drugs in wastewater by mixed-mode solid-phase extraction and quadrupole-time-of-flight liquid chromatography-mass spectrometry. Anal Chem. 2012;84(3):1708-17.
González-Mariño, I., Quintana, J. B., Rodríguez, I., González-Díez, M., & Cela, R. (2012). Screening and selective quantification of illicit drugs in wastewater by mixed-mode solid-phase extraction and quadrupole-time-of-flight liquid chromatography-mass spectrometry. Analytical Chemistry, 84(3), 1708-17. https://doi.org/10.1021/ac202989e
González-Mariño I, et al. Screening and Selective Quantification of Illicit Drugs in Wastewater By Mixed-mode Solid-phase Extraction and Quadrupole-time-of-flight Liquid Chromatography-mass Spectrometry. Anal Chem. 2012 Feb 7;84(3):1708-17. PubMed PMID: 22185484.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Screening and selective quantification of illicit drugs in wastewater by mixed-mode solid-phase extraction and quadrupole-time-of-flight liquid chromatography-mass spectrometry. AU - González-Mariño,Iria, AU - Quintana,José Benito, AU - Rodríguez,Isaac, AU - González-Díez,Marta, AU - Cela,Rafael, Y1 - 2012/01/12/ PY - 2011/12/22/entrez PY - 2011/12/22/pubmed PY - 2012/6/19/medline SP - 1708 EP - 17 JF - Analytical chemistry JO - Anal Chem VL - 84 IS - 3 N2 - For the first time, a mixed-mode solid-phase extraction with fractionation of basic analytes from neutral and acidic species during cartridge elution and liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) was combined for the quantitative determination of 24 illicit drugs and metabolites in urban sewage samples. The effects of several sample preparation and instrumental parameters in the sensitivity and selectivity of the quantitative method are thoroughly discussed. Under final working conditions, recoveries above 63% and 82% were attained for all species in raw and treated sewage, respectively; whereas, the limits of quantification of the method, defined for a signal-to-noise of 10 (S/N = 10), ranged from 2 to 50 ng L(-1). Sequential elution of mixed-mode cartridges allowed a significant reduction of matrix effects observed during electrospray ionization of basic drugs versus those measured for hydrophilic balance reversed-phase sorbents and the same mixed-mode polymer without fractionated elution. Analysis of raw wastewater samples confirmed the ubiquity of cocaine (COC), benzoylecgonine (BE), and 11-nor-9-carboxy-Δ(9)-tetrahydrocannabinol (THCCOOH) in this matrix. The capability of the above methodology to identify new illicit drugs and/or metabolites in sewage samples is also discussed. With this aim, a two step strategy is proposed. First, high-resolution MS chromatograms, acquired throughout each chromatographic run, are automatically searched against an in-house built database, a reduced list of candidate drugs is generated, and the corresponding extracted ion chromatograms are obtained. In a further LC run, the tandem mass spectrometry (MS/MS) spectra of unknown peaks are acquired using different collision energies and compared with those existing in public libraries, or interpreted, to assign the unknown peak to one of the previously selected candidates. SN - 1520-6882 UR - https://www.unboundmedicine.com/medline/citation/22185484/Screening_and_selective_quantification_of_illicit_drugs_in_wastewater_by_mixed_mode_solid_phase_extraction_and_quadrupole_time_of_flight_liquid_chromatography_mass_spectrometry_ L2 - https://doi.org/10.1021/ac202989e DB - PRIME DP - Unbound Medicine ER -