A systematic strategy for the identification and determination of pharmaceuticals in environment using advanced LC-MS tools: application to ground water samples.
In the present study, a novel analytical strategy was employed to study the occurrence of 40 drug residues belonging to different medicinal classes, e.g., antibiotics, β blockers, NSAIDs, antidiabetics, proton pump inhibitors, H2 receptor antagonists, antihypertensives, antihyperlipidemics, etc. in ground water samples collected from villages adjoining to S.A.S. Nagar, Punjab, India. The drug residues were extracted from the samples using solid-phase extraction, and LC-ESI-HRMS and LC-ESI-MS/MS were used for identification and quantitation of the analytes. Initially, qualifier and quantifier MRM transitions were classified for 40 targeted drugs, followed by development of LC-MS methods for the separation of all the drugs, which were divided into three categories to curtail overlapping of peaks. Overall identification was done through matching of retention times and MRM transitions; matching of intensity ratio of qualifier to quantifier transitions; comparison of base peak MS/MS profiles; and evaluation of isotopic abundances (wherever applicable). Final confirmation was carried out through comparison of accurate masses obtained from HRMS studies for both standard and targeted analytes in the samples. The application of the strategy allowed removal of false positives and helped in identification and quantitation of diclofenac in the ground water samples of four villages, and pitavastatin in a sample of one village.
Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research (NIPER), Sector 67, S.A.S. Nagar, 160062 Punjab, India.
Kriti
K
Jindal
Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research (NIPER), Sector 67, S.A.S. Nagar, 160062 Punjab, India.
Mallikarjun
M
Narayanam
Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research (NIPER), Sector 67, S.A.S. Nagar, 160062 Punjab, India. Electronic address: ssingh@niper.ac.in.
Saranjit
S
Singh
D002853:Chromatography, Liquid / Q000379:methods*; D004784:Environmental Monitoring / Q000379:methods; D060587:Groundwater / Q000032:analysis* / Q000737:chemistry; D007194:India; D013058:Mass Spectrometry / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry
D004364:Pharmaceutical Preparations; D014874:Water Pollutants, Chemical
Analytical strategy; Drugs; Environment; Ground water; LC–MS