title: Determination of Urinary PAH Metabolites Using DLLME Hyphenated to Injector Port Silylation and GC-MS-MS.
abstract: Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous environmental pollutants and well-known carcinogens. Hydroxy derivatives of PAH are considered as biomarkers of PAH exposure, and there is a need to measure these metabolites at low concentrations. So, a precise and eco-friendly analytical method has been developed for rapid determination of PAH metabolites. For the first time, a new analytical method based on coupling of dispersive liquid-liquid microextraction (DLLME) with auto-injector port silylation (auto-IPS) followed by gas chromatography-tandem mass spectrometry (GC-MS-MS) analysis is reported for the analysis of seven urinary PAH metabolites. Factors affecting DLLME and IPS, such as type and volume of extraction and disperser solvent, pH, ionic strength, injector port temperature, volume of N,O-bis(trimethylsilyl)trifluoroacetamide and type of solvent were investigated. Under optimized conditions, the limit of detection and limit of quantification were found to be in the range of 1-9 and 3-29 ng/mL, respectively. Satisfactory recoveries of metabolites in urine samples in the range of 87-95% were found. The developed method has been successfully applied for the determination of PAH metabolites in urine samples of exposed workers. DLLME-auto-IPS-GC-MS-MS method is time, labor, solvent and reagent saving, which can be routinely used for the analysis of urinary PAH metabolites.
authors.affiliation: Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India.
authors.forename: Manoj Kumar
authors.initials: MK
authors.lastname: Gupta
authors.affiliation: Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India.
authors.forename: Rajeev
authors.initials: R
authors.lastname: Jain
authors.affiliation: Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India.
authors.forename: Pratibha
authors.initials: P
authors.lastname: Singh
authors.affiliation: Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India.
authors.forename: Ratnasekhar
authors.initials: R
authors.lastname: Ch
authors.affiliation: Academy of Scientific and Innovative Research (AcSIR), CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research (CSIR-IITR), PO Box 80, MG Marg, Lucknow 226001, India mohanitrc@gmail.com mmudiam@iitr.res.in.
authors.forename: Mohana Krishna Reddy
authors.initials: MK
authors.lastname: Mudiam
mesh_terms: D015415:Biomarkers / Q000652:urine; D001711:Biotransformation; D002021:Buffers; D002138:Calibration; D004784:Environmental Monitoring / Q000592:standards; D008401:Gas Chromatography-Mass Spectrometry / Q000592:standards; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000592:standards; D016273:Occupational Exposure; D009994:Osmolar Concentration; D011084:Polycyclic Aromatic Hydrocarbons / Q000652:urine*; D012015:Reference Standards; D015203:Reproducibility of Results; D012821:Silanes / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000592:standards
chemical_list: D015415:Biomarkers; D002021:Buffers; D011084:Polycyclic Aromatic Hydrocarbons; D012821:Silanes