Method for detecting aldicarb and metabolite of aldicarb in fruits and vegetables through graphene oxide dispersive solid-phase extraction

A technology for dispersing solid phase and graphene, which is applied in the field of analytical chemistry detection to achieve the effects of low cost, reduced sample matrix interference, and simple method operation.

Inactive Publication Date: 2016-06-29
JINING ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF P R C
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  • Abstract
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Problems solved by technology

Graphene oxide as a dispersive phase extraction adsorbent for the detection of aldicarb and its metabolite residues in fruits and vegetables has not been reported

Method used

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  • Method for detecting aldicarb and metabolite of aldicarb in fruits and vegetables through graphene oxide dispersive solid-phase extraction
  • Method for detecting aldicarb and metabolite of aldicarb in fruits and vegetables through graphene oxide dispersive solid-phase extraction
  • Method for detecting aldicarb and metabolite of aldicarb in fruits and vegetables through graphene oxide dispersive solid-phase extraction

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Embodiment Construction

[0021] Take apple detection as an example to illustrate the present invention.

[0022] equipment:

[0023] 1290-6460 liquid chromatography-tandem mass spectrometer from Agilent of the United States, equipped with jet stream ion focusing electrospray ion source (AJS-ESI); GM200 high-speed homogenizer from IKA, Germany; MMV-1000W oscillator from Tokyo, Japan; CR22GⅢ high-speed refrigerated centrifuge from Hitachi, Japan; R215 rotary evaporator from Buchi, Switzerland; MS3 vortex mixer from IKA, Germany.

[0024] Materials and Reagents:

[0025] Graphene oxide was provided by Jining Lite Nano Technology Co., Ltd.; acetonitrile, methanol, and formic acid were all chromatographically pure; anhydrous sodium sulfate (burned at 650°C for 4 hours, stored in a desiccator after cooling, for use), and sodium chloride were Analytical pure; experimental water is ultrapure water.

[0026] Standard products: Aldicarb, aldicarb sulfone, and aldicarb sulfoxide standard products are all 100m...

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Abstract

The invention discloses a method for detecting aldicarb and its metabolites in fruits and vegetables by graphene oxide dispersed solid-phase extraction, which belongs to the field of analytical chemistry detection. The method includes the following steps: (1) Extraction: Weigh the sample into a 50ml centrifuge tube, add acetonitrile, homogenize for 1min, then add 4g of anhydrous sodium sulfate and 1g of sodium chloride, shake and centrifuge to collect the supernatant in pears Concentrate to dryness by rotary evaporation in a water bath at 40°C. (2) Purification: Dissolve the residue with acetonitrile-0.1% formic acid aqueous solution, transfer to a 15mL centrifuge tube, add graphene oxide, vortex, stand still, and pass through a 0.22μm organic phase filter membrane. (3) Detection: The sample liquid after the filter membrane is detected by liquid chromatography-tandem mass spectrometry (LC-MS / MS). The beneficial effect of the present invention is that a simple and rapid detection method for aldicarb and its metabolites is established by utilizing graphene oxide dispersive solid-phase extraction technology, the method is simple to operate, low in cost, can reduce sample matrix interference, and is suitable for fruits and vegetables detection.

Description

technical field [0001] The invention relates to a method for detecting aldicarb and its metabolites in fruits and vegetables by graphene oxide dispersive solid phase extraction, in particular to a method for detecting aldicarb and its metabolites in fruits and vegetables by graphene oxide dispersive solid phase extraction combined with liquid chromatography tandem mass spectrometry. A method for metabolite residues belongs to the field of analytical chemistry detection. Background technique [0002] Aldicarb is a highly efficient and highly toxic carbamate insecticide, which is widely used in the field of fruit and vegetable cultivation. Aldicarb is easily oxidized into more toxic metabolites, aldicarb sulfone, Aldicarb sulfoxide. Due to its high efficiency and economy, it is widely used in the process of growing fruits and vegetables, and the resulting drug residues and poisoning incidents of aldicarb and its metabolites occur from time to time. At present, the commonly u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 倪永付
Owner JINING ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF P R C
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