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一种由二氧化硅、石墨烯和钯(II)组成的中孔纳米吸附剂,用于在离子淌度谱法定量分析前通过超声辅助分散固相萃取有机磷农药。

A mesoporous nanosorbent composed of silica, graphene, and palladium (II) for ultrasound-assisted dispersive solid-phase extraction of organophosphorus pesticides prior to their quantitation by ion mobility spectrometry.

机构信息

Faculty of Chemistry, Shahid Beheshti University, G. C., P.O. Box 1983963113, Evin, Tehran, Islamic Republic of Iran.

出版信息

Mikrochim Acta. 2020 Mar 9;187(4):209. doi: 10.1007/s00604-020-4174-2.

DOI:10.1007/s00604-020-4174-2
PMID:32152680
Abstract

A new ultrasonic-assisted dispersive solid-phase extraction method using mesoporous nanosorbent composed of silica, graphene, and palladium (II) (M S/G@-SH@Pd (II)), coupled with corona discharge ion mobility spectrometry, was developed for trace determination of organophosphorus pesticides. Initially, the M S/G@-SH@Pd (II) nanosorbent was synthesized and characterized. Then, the nanosorbent was used for the sorption and extraction of organophosphorus pesticides. Under the optimized conditions (pH = 7.0, 15 mg of sorbent, 3 min extraction time, ethanol as desorption agent, 3 min centrifuge time), the proposed technique provided good linearity (R > 0.994), repeatability (RSD < 4.6%), low limits of detection (0.15-0.30 ng mL), excellent preconcentration factor (PF = 472-478), and high recoveries (93-94%). The method was applied to the determination of organophosphorus pesticides in real water samples. The sorbent was reused in 5 cycles without any considerable loss of activity. Graphical abstract Schematic presentation of design and synthesis of mesoporous nanosorbent composed of silica, graphene, and palladium (II) for ultrasound-assisted dispersive solid-phase extraction of organophosphorus pesticides prior to their quantitation by ion mobility spectrometry.

摘要

一种新的超声辅助分散固相萃取方法,使用由二氧化硅、石墨烯和钯(II)组成的中孔纳米吸附剂(M S/G@-SH@Pd (II)),与电晕放电离子淌度谱联用,用于痕量测定有机磷农药。首先合成并表征了 M S/G@-SH@Pd (II)纳米吸附剂。然后,纳米吸附剂用于有机磷农药的吸附和萃取。在优化条件下(pH=7.0,15 mg 吸附剂,3 min 萃取时间,乙醇作为洗脱剂,3 min 离心时间),提出的技术提供了良好的线性(R>0.994)、重复性(RSD<4.6%)、低检测限(0.15-0.30 ng mL)、出色的浓缩因子(PF=472-478)和高回收率(93-94%)。该方法应用于实际水样中有机磷农药的测定。吸附剂在没有明显活性损失的情况下可重复使用 5 次。

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本文引用的文献

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2
Applications of three-dimensional graphenes for preconcentration, extraction, and sorption of chemical species: a review.三维石墨烯在化学物质预富集、萃取和吸附中的应用:综述
Mikrochim Acta. 2019 Mar 9;186(4):232. doi: 10.1007/s00604-019-3324-x.
3
Ultrasound assisted dispersive solid phase extraction of triazole fungicides by using an N-heterocyclic carbene copper complex supported on ionic liquid-modified graphene oxide as a sorbent.
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4
Hybrid nanocomposites prepared from a metal-organic framework of type MOF-199(Cu) and graphene or fullerene as sorbents for dispersive solid phase extraction of polycyclic aromatic hydrocarbons.由 MOF-199(Cu) 型金属有机骨架和石墨烯或富勒烯制备的杂化纳米复合材料,作为多环芳烃分散固相萃取的吸附剂。
Mikrochim Acta. 2019 Feb 1;186(3):131. doi: 10.1007/s00604-019-3246-7.
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