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Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry.
J Chromatogr A. 2011 Apr 22; 1218(16):2264-75.JC

Abstract

A multi-class method for the simultaneous quantification and confirmation of 47 pharmaceuticals in environmental and wastewater samples has been developed. The target list of analytes included analgesic and anti-inflammatories, cholesterol lowering statin drugs and lipid regulators, antidepressants, anti-ulcer agents, psychiatric drugs, ansiolitics, cardiovasculars and a high number (26) of antibiotics from different chemical groups. A common pre-concentration step based on solid-phase extraction with Oasis HLB cartridges was applied, followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) measurement. All compounds were satisfactorily determined in just one single injection, with a chromatographic run time of only 10 min. The process efficiency (combination of the matrix effect and the extraction process recovery) for the 47 selected compounds was evaluated in nine effluent wastewater (EWW) samples, and the use of different isotope-labelled internal standards (ILIS) was investigated to correct unsatisfactory values. Up to 12 ILIS were evaluated in EWW and surface water (SW). As expected, the ILIS provided satisfactory correction for their own analytes. However, the use of these ILIS for the rest of pharmaceuticals was problematic in some cases. Despite this fact, the correction with analogues ILIS was found useful for most of analytes in EWW, while was not strictly required in the SW tested. The method was successfully validated in SW and EWW at low concentration levels, as expected for pharmaceuticals in these matrices (0.025, 0.1 and 0.5 μg/L in SW; 0.1 and 0.5 μg/L in EWW). With only a few exceptions, the instrumental limits of detection varied between 0.1 and 8 pg. The limits of quantification were estimated from sample chromatograms at the lowest spiked levels tested and normally were below 20 ng/L for SW and below 50 ng/L for EWW. The developed method was applied to the analysis of around forty water samples (river waters and effluent wastewaters) from the Spanish Mediterranean region. Almost all the pharmaceuticals selected in this work were detected, mainly in effluent wastewater. In both matrices, analgesics and anti-inflammatories, lipid regulators and quinolone antibiotics were the most detected groups.

Authors+Show Affiliations

Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.No affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

21388627

Citation

Gracia-Lor, Emma, et al. "Multi-class Determination of Around 50 Pharmaceuticals, Including 26 Antibiotics, in Environmental and Wastewater Samples By Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry." Journal of Chromatography. A, vol. 1218, no. 16, 2011, pp. 2264-75.
Gracia-Lor E, Sancho JV, Hernández F. Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry. J Chromatogr A. 2011;1218(16):2264-75.
Gracia-Lor, E., Sancho, J. V., & Hernández, F. (2011). Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry. Journal of Chromatography. A, 1218(16), 2264-75. https://doi.org/10.1016/j.chroma.2011.02.026
Gracia-Lor E, Sancho JV, Hernández F. Multi-class Determination of Around 50 Pharmaceuticals, Including 26 Antibiotics, in Environmental and Wastewater Samples By Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry. J Chromatogr A. 2011 Apr 22;1218(16):2264-75. PubMed PMID: 21388627.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry. AU - Gracia-Lor,Emma, AU - Sancho,Juan V, AU - Hernández,Félix, Y1 - 2011/02/18/ PY - 2010/11/02/received PY - 2011/02/09/revised PY - 2011/02/10/accepted PY - 2011/3/11/entrez PY - 2011/3/11/pubmed PY - 2011/7/12/medline SP - 2264 EP - 75 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1218 IS - 16 N2 - A multi-class method for the simultaneous quantification and confirmation of 47 pharmaceuticals in environmental and wastewater samples has been developed. The target list of analytes included analgesic and anti-inflammatories, cholesterol lowering statin drugs and lipid regulators, antidepressants, anti-ulcer agents, psychiatric drugs, ansiolitics, cardiovasculars and a high number (26) of antibiotics from different chemical groups. A common pre-concentration step based on solid-phase extraction with Oasis HLB cartridges was applied, followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) measurement. All compounds were satisfactorily determined in just one single injection, with a chromatographic run time of only 10 min. The process efficiency (combination of the matrix effect and the extraction process recovery) for the 47 selected compounds was evaluated in nine effluent wastewater (EWW) samples, and the use of different isotope-labelled internal standards (ILIS) was investigated to correct unsatisfactory values. Up to 12 ILIS were evaluated in EWW and surface water (SW). As expected, the ILIS provided satisfactory correction for their own analytes. However, the use of these ILIS for the rest of pharmaceuticals was problematic in some cases. Despite this fact, the correction with analogues ILIS was found useful for most of analytes in EWW, while was not strictly required in the SW tested. The method was successfully validated in SW and EWW at low concentration levels, as expected for pharmaceuticals in these matrices (0.025, 0.1 and 0.5 μg/L in SW; 0.1 and 0.5 μg/L in EWW). With only a few exceptions, the instrumental limits of detection varied between 0.1 and 8 pg. The limits of quantification were estimated from sample chromatograms at the lowest spiked levels tested and normally were below 20 ng/L for SW and below 50 ng/L for EWW. The developed method was applied to the analysis of around forty water samples (river waters and effluent wastewaters) from the Spanish Mediterranean region. Almost all the pharmaceuticals selected in this work were detected, mainly in effluent wastewater. In both matrices, analgesics and anti-inflammatories, lipid regulators and quinolone antibiotics were the most detected groups. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/21388627/Multi_class_determination_of_around_50_pharmaceuticals_including_26_antibiotics_in_environmental_and_wastewater_samples_by_ultra_high_performance_liquid_chromatography_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(11)00241-X DB - PRIME DP - Unbound Medicine ER -