Determination of 89 drugs and other micropollutants in unfiltered wastewater and freshwater by LC-MS/MS: an alternative sample preparation approach

Anal Bioanal Chem. 2017 Oct;409(26):6205-6225. doi: 10.1007/s00216-017-0561-x. Epub 2017 Aug 16.

Abstract

A liquid chromatography-triple quadrupole-tandem mass spectrometry (LC-qQq-MS/MS) method was developed for simultaneous determination of 89 legal neuropsychiatric pharmaceuticals and illicit drugs (both parent compounds and metabolites) and other micropollutants in unfiltered wastewater and freshwater. The target chemicals fall under the classes of amphetamine-type stimulants, cocaine compounds, opiates and opioids, benzodiazepines, lysergic compounds, antipsychotics, anesthetics, antiepileptics, antidepressants, sympathomimetics, cannabinoids, blood thinners, antihistamines, β-blockers, caffeine derivatives, nicotine derivatives, z-drugs, new designer drugs, and Alzheimer medications. The sample preparation procedure was designed for unfiltered wastewater and freshwater without the need to separate the particulate matter (if any) from the aqueous phase prior to extraction. Samples were pre-concentrated by rotary evaporation in the presence of a solvent. Method precision (absolute values; N = 6 replicate analyses at the fortification level of 50 ng, k = 6 days) for 87 out of 89 target analytes ranged from 2.8 to 34% (RSD %). The limits of detection ranged from 0.11 to 202 ng L-1, and the matrix effects ranged from +16 to -84%. A total of 10 samples, 8 wastewater, 1 drinking water, and 1 lake water, were collected from New York State, USA, and were analyzed for the target compounds to demonstrate the applicability of the developed method. This is the first study to report the analysis of multiple classes of pharmaceuticals, illicit drugs, and other micropollutants in unfiltered wastewater. Graphical abstract Analysis of 89 micropollutants in unfiltered wastewater by LC-MS/MS.

Keywords: Drugs; Freshwater; Illicit drugs; Micropollutants; Narcotics; Wastewater.

Publication types

  • Evaluation Study

MeSH terms

  • Chromatography, Liquid / methods*
  • Fresh Water / analysis*
  • Illicit Drugs / analysis
  • Limit of Detection
  • Pharmaceutical Preparations / analysis*
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / methods*
  • Wastewater / analysis*
  • Water Pollutants, Chemical / analysis*

Substances

  • Illicit Drugs
  • Pharmaceutical Preparations
  • Waste Water
  • Water Pollutants, Chemical