title: Evaluation of layered double hydroxide/graphene hybrid as a sorbent in membrane-protected stir-bar supported micro-solid-phase extraction for determination of organochlorine pesticides in urine samples.
abstract: In this work, the potential of layered double hydroxide/graphene (LDH-G) hybrid as a sorbent for extraction and preconcentration of fifteen organochlorine pesticides (OCPs) in urine samples was evaluated. The LDH-G hybrid was synthesized by co-precipitation method and it was then characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The sorbent was then employed in membrane-protected stir-bar supported micro-solid-phase extraction (SB-μ-SPE) of OCPs in urine samples. This extraction approach is highly suitable for the samples representing matrix complexity such as urine because the sorbent is effectively protected inside the membrane. The extracted samples were analyzed by gas chromatography mass spectrometry. The factors that affect the performance of SB-μ-SPE were suitably optimized. This method demonstrated good linearity with coefficients of determination up to 0.9996. The limits of detection ranged between 0.22 and 1.38ngmL-1. The RSD values for intra and inter-day precision were also in a satisfactory range (2.7-9.5%).
authors.affiliation: Center for Environment and Water (CEW), Research Institute, King Fahd University of Petroleum and Minerals (KFUPM), Dhahran 31261, Saudi Arabia. Electronic address: msajid@kfupm.edu.sa.
authors.forename: Muhammad
authors.initials: M
authors.lastname: Sajid
authors.affiliation: Department of Chemistry, 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 Chemical Engineering, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia.
authors.forename: Muhammad
authors.initials: M
authors.lastname: Daud
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
mesh_terms: D004785:Environmental Pollutants / Q000302:isolation & purification / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry; D006108:Graphite / Q000737:chemistry*; D006801:Humans; D006843:Hydrocarbons, Chlorinated / Q000302:isolation & purification / Q000652:urine*; D006878:Hydroxides / Q000737:chemistry; D010575:Pesticides / Q000302:isolation & purification / Q000652:urine*; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D004785:Environmental Pollutants; D006843:Hydrocarbons, Chlorinated; D006878:Hydroxides; D010575:Pesticides; D006108:Graphite
keywords: Biological analysis; Layered double hydroxide/graphene hybrid; Membrane-protected stir-bar supported micro-solid-phase extraction; Microextraction; Organochlorine pesticides; Persistent organic pollutants