Graphitic carbon nitride as sorbent for the emulsification-enhanced disposable pipette extraction of eight organochlorin
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ORIGINAL PAPER
Graphitic carbon nitride as sorbent for the emulsification-enhanced disposable pipette extraction of eight organochlorine pesticides prior to GC-MS analysis Sze Chieh Tan 1,2
&
Hian Kee Lee 1,2
Received: 17 September 2019 / Accepted: 30 December 2019 # Springer-Verlag GmbH Austria, part of Springer Nature 2020
Abstract Graphitic carbon nitride (g-C3N4) was explored as a sorbent for the emulsification-enhanced (EE) disposable pipette extraction (DPX) of eight organochlorine pesticides (OCPs) from environmental waters. The OCPs, including α-hexachlorocyclohexane, Aldrin, α-Chlordane, Dieldrin, 4,4′-dichlorodiphenyldichloroethylene, 4,4′-dichlorodiphenyldichloroethane, Heptachlor and Heptachlor epoxide (Isomer A), were analyzed by gas chromatography-mass spectrometry. The sorbent g-C3N4 was characterized by elemental analysis, X-ray diffraction, scanning electron microscopy, Fourier-transform infrared and Raman spectroscopy. As a C-N analogue of graphite, g-C3N4 exhibits good water dispersibility and allows easy analyte recovery – a characteristic not commonly observed in carbon-based materials. When applied to DPX, g-C3N4 rapidly establishes strong interactions with the OCPs. Consequently, g-C3N4 displays superior extraction capability in comparison to six other commercial sorbents. An emulsification step prior to DPX was found to enhance the overall extraction efficiency by pre-concentrating the OCPs into the microdroplets of an organic solvent. The microdroplets were then adsorbed onto g-C3N4. Under the most favorable conditions, wide linear responses spanning over two to four orders of magnitudes are established. The limits of detection range between 2.4 ng·L−1 and 46.2 ng·L−1. The method is reproducible (relative standard deviations ≤ 7.4%) and enrichment factors are between 42 and 57. When applied to the analysis of lake and river water samples, EE-DPX-gas chromatography-mass spectrometry exhibits good resilience against matrix interferences. The relative recoveries range between 77.7% and 106.3%. In comparison to other sorbent-based extraction techniques reported for the analysis of OCPs in aqueous samples, EE-DPX utilizes the minimal amount of sample and solvent, and requires the shortest sample preparation time.
Keywords Bulk material . g-C3N4 . Sample preparation . Microextraction . Sorbent-based extraction . Large volume injection . Gas chromatography-mass spectrometry . Halogenated compounds . Environmental water analysis
Introduction
Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00604-019-4107-0) contains supplementary material, which is available to authorized users. * Hian Kee Lee [email protected] 1
NUS Graduate School for Integrative Sciences and Engineering, National University of Singapore, University Hall, Tan Chin Tuan Wing #04-02, 21 Lower Kent Ridge Road, Singapore 119077, Singapore
2
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore
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