title: Single-step microwave assisted headspace liquid-phase microextraction of trihalomethanes and haloketones in biological samples.
abstract: A single-step microwave assisted headspace liquid-phase microextraction (MA-HS-LPME) method was developed for determination of trihalomethanes (THMs) and haloketones (HKs) in biological samples. In this method, a porous membrane envelope was filled with few microliters of extraction solvent and then placed inside the microwave extraction vial. A PTFE ring was designed to support the membrane envelope over a certain height inside the vial. An optimum amount of biological sample was placed in the vial equipped with magnetic stirrer. After that nitric acid was added to the vial for digestion of biological sample. The sample was digested and the volatile THMs and HKs were extracted at headspace in the solvent containing porous membrane. After simultaneous digestion and extraction, the extract was injected to gas chromatography/mass spectrometry for analysis. Factors affecting the extraction efficiency were optimized to achieve higher extraction performance. Quantification was carried out over a concentration range of 0.3-100ngg(-1) for brominated compounds while for the chlorinated ones linear range was between 0.5-100ngg(-1). Limit of detections (LODs) were ranged from 0.051 to 0.110ngg(-1) while limit of quantification (LOQ) were in the range of 0.175-0.351ngg(-1). The relative standard deviations (RSDs) of the calibrations were ranged between 1.1 and 6.8%. The MA-HS-LPME was applied for the determination of trace level THMs and HKs in fish tissue and green alga samples.
authors.affiliation: Department of Chemistry, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia.
authors.forename: Abdulnaser
authors.initials: A
authors.lastname: Alsharaa
authors.affiliation: Department of Chemistry, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia; Center of Excellence in Nanotechnology, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia. Electronic address: cbasheer@kfupm.edu.sa.
authors.forename: Chanbasha
authors.initials: C
authors.lastname: Basheer
authors.affiliation: Department of Chemistry, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia.
authors.forename: Muhammad
authors.initials: M
authors.lastname: Sajid
mesh_terms: D000818:Animals; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry; D007659:Ketones / Q000032:analysis*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D008872:Microwaves; D022882:Trihalomethanes / Q000032:analysis*
chemical_list: D007659:Ketones; D022882:Trihalomethanes
keywords: Disinfection by-products; Environmental applications; Gas chromatography–; Microwave assisted headspace liquid-phase microextraction; mass spectrometry