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A kind of electrochemical reduction graphene oxide solid-phase microextraction fiber preparation method

A technology for extracting fibers and graphene, which is applied in the field of preparation of electrochemically reduced graphene oxide solid-phase microextraction fibers, can solve the problems of weak coating stability and poor reproducibility, and achieve strong adsorption capacity, thermal stability and chemical stability. Good stability and large specific surface area

Active Publication Date: 2021-01-29
JIANGNAN UNIV
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  • Abstract
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Problems solved by technology

At present, the commonly used coating preparation methods include sol-gel method, physical coating method, covalent bonding method, etc. However, these preparation methods have the disadvantages of poor reproducibility and weak coating stability.

Method used

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  • A kind of electrochemical reduction graphene oxide solid-phase microextraction fiber preparation method
  • A kind of electrochemical reduction graphene oxide solid-phase microextraction fiber preparation method
  • A kind of electrochemical reduction graphene oxide solid-phase microextraction fiber preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: the preparation of solid phase microextraction fiber

[0050] (1) Preparation of graphene oxide electrolyte: ultrasonically disperse 30 mg of graphene oxide powder in 10 mL of distilled water to obtain a graphene oxide aqueous solution with a concentration of 3 mg / mL, and add 0.1225 g of NaClO to the dispersion 4 , NaClO 4The concentration is 0.1mol / L, and the graphene oxide electrolyte is obtained after mixing evenly.

[0051] (2) Electrochemical deposition: corrode the lower end 2 cm of the stainless steel wire with aqua regia for 15 minutes, wash it with distilled water, and use it as a working electrode for later use. A CHI660C electrochemical workstation was used, the corroded stainless steel wire was used as the working electrode, the saturated calomel electrode was used as the reference electrode, and the platinum electrode was used as the counter electrode. Using the constant potential method, apply a voltage of -1.2V and keep it for 200-600 seco...

Embodiment 2

[0057] Embodiment 2: Optimization of solid-phase microextraction conditions

[0058] In this experiment, the conditions of solid-phase microextraction were optimized.

[0059] Add benzo[a]pyrene standard working solution to the barbecue supernatant, dilute to 10mL with distilled water, so that the concentration of benzo[a]pyrene is 50ng / mL. Different extraction temperature (40, 50, 60, 70, 80°C), extraction time (10, 20, 30, 40, 50min), stirring rate (100, 300, 500, 700, 900rpm) and desorption time ( 1, 2, 3, 4, 5min) such as Figure 7 , Figure 8 , Figure 9 , Figure 10 As shown, the conditions for a better enrichment and extraction effect are: 70°C as the extraction temperature, 30 min as the extraction time, a stirring rate of 700 rpm, and a desorption time of 4 min.

Embodiment 3

[0060] Example 3: SPME-GC enrichment detection of benzo[a]pyrene in barbecue

[0061] (1) Preparation of standard solution

[0062] Dissolve 1 mg of benzo[a]pyrene standard powder in 10 mL of acetone to prepare a 100 mg / L benzo[a]pyrene stock solution, and dilute the stock solution to 10 mg / L as an intermediate solution. The concentration of the standard curve working solution is 0.05ng / mL, 0.1ng / mL, 0.5ng / mL, 1ng / mL, 5ng / mL, 10ng / mL, 100ng / mL, 200ng / mL.

[0063] (2) Sample pretreatment

[0064] Accurately weigh 2g of roast meat into a centrifuge tube, add 5mL of acetone, ultrasonically extract for 40min, centrifuge at 10000rpm for 10min, and take the supernatant; add 5mL of acetone again, repeat the ultrasonication and centrifugation operations, and combine the supernatant twice.

[0065] (3) SPME combined with GC

[0066] Dilute 50 μL of barbecue supernatant with distilled water into a 10 mL extraction vial, put a stirring bar, insert self-made solid-phase microextraction...

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Abstract

The invention discloses a method for preparing electrochemically reduced graphene oxide solid-phase microextraction fibers, which belongs to the technical field of food safety detection. The invention provides a preparation method of electrochemically reduced graphene oxide solid-phase microextraction fiber, which uses graphene oxide to undergo a reduction reaction at a negative potential, and deposits a reduced graphene oxide coating on a metal wire working electrode for extraction Benzo[a]pyrene in food, combined with gas chromatography for detection. The method of the invention is simple and fast, and the thickness of the coating can be freely controlled by the deposition time. At the same time, combined with the advantages of large specific surface area and strong adsorption capacity of graphene, the work efficiency of solid-phase microextraction is greatly improved.

Description

technical field [0001] The invention relates to a method for preparing electrochemically reduced graphene oxide solid-phase microextraction fibers, which belongs to the technical field of food safety detection. Background technique [0002] Solid-phase microextraction (solid-phase microextraction, SPME) is an extraction and enrichment technique that is easy to operate and does not require a large amount of solvent. Because of its simplicity and convenience, and the advantages of integrating separation, enrichment and detection, it has been widely used in the field of food testing. Some commercial SPME fibers have some limitations, such as the quartz substrate is easy to break, poor thermal and chemical stability, and expensive. Therefore, it is necessary to prepare a solid-phase microextraction fiber with stable properties and high mechanical strength. The core of SPME technology is the extraction coating. The properties of the coating are not only related to the physical ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 沈晓芳郭思依杨成庞月红
Owner JIANGNAN UNIV
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