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

• Published in: Journal of Chromatography A 2017-03, Vol.1489, p.1-8
• Main Authors: Sajid, Muhammad, Basheer, Chanbasha, Daud, Muhammad, Alsharaa, Abdulnaser
• Format: Article
• Language: English
• Subjects: Biological analysis; Layered double hydroxide/graphene hybrid; Membrane-protected stir-bar supported micro-solid-phase extraction; Microextraction; Organochlorine pesticides; Persistent organic pollutants
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2017.01.089

•For the first time, layered double hydroxide/graphene hybrid was employed as sorbent in SB-μ-SPE.•Fifteen organochlorine pesticides were analyzed in urine samples.•Factors that affect extraction performance were suitably optimized.•This method provided good linear range and limits of detection. 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%).