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Electrically-driven solid phase micro-extraction method and device thereof

A solid-phase microextraction column and electric-driven technology, which is applied in the field of electric-driven solid-phase microextraction and its devices, can solve the problems of adsorption and extraction of various target analytes, damage of solid-phase microextraction fiber head, unfavorable double Electric layer generation and other issues, to achieve the effect of improving analysis and detection sensitivity, easy assembly and adjustment, and easy operation

Inactive Publication Date: 2015-04-15
NINGBO UNIV
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Problems solved by technology

[0005] Although the above work has proved that applying an electric field can accelerate the extraction rate of solid-phase microextraction and increase the extraction capacity, there are still the following relative deficiencies: (1) most of the electric double layer of the porous electrode is not formed on the electrode surface, but It is formed in the pores, and the pore diameter of the more porous electrodes is not much different from the thickness of the electric double layer in the order of magnitude, that is, when it is equal to or less than 10nm, because the pore diameter is too small, the "overlapping effect" will occur in the space. "(Yin Guangjun, Chen Fuming, Water Treatment Technology, 2003, 29(2), 63-65) is not conducive to the formation of electric double layer
(2) The existing electro-adsorption materials are mainly various C-based materials, which are single in variety and difficult to absorb and extract a variety of target analytes.
(3) The higher the applied voltage, the faster the adsorption rate increases, and the applied voltage in the existing electrosorption process is mostly within a few volts, which limits the increase of the adsorption rate to a certain extent.
(4) In the existing electrosorption solid-phase microextraction technology, the method of increasing the mass transfer rate by using a magnetic stirrer to stir the solution will also be limited, especially when the solution volume is very small. In addition, using Magnetic stirring is easy to cause damage to the fiber head of solid phase microextraction

Method used

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  • Electrically-driven solid phase micro-extraction method and device thereof
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preparation Embodiment 1

[0036] 1) Pretreatment of metal wire 2: Take a section of stainless steel wire (30mm×1.2mm i.d.) and clean it. After drying, apply a thin layer with a commercially available epoxy resin adhesive, and wait until it is fully cured.

[0037] 2) Preparation of solid phase microextraction column 3: Take 4.0g PEG-1540 and heat it to melt, add 2.0g epoxy resin and mix for 2min, after cooling to room temperature, add 0.5g diethylenetriamine, and mix thoroughly for 2min Obtain a uniform and transparent viscous liquid, pour it into a 1mL disposable syringe (polypropylene material, tube inner diameter about 5mm), inject the liquid with a length of about 10-15mm, and immerse the aforementioned treated stainless steel wire 2 vertically into the reaction In the liquid, leave a section outside the reaction solution, seal it and place it in an oven at 60° C. for reaction for 24 hours, and take the prepared solid phase micro extraction column 3 out of the container.

[0038] 3) Post-treatment of th...

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Abstract

The invention relates to an electrically-driven solid phase micro-extraction method and a device thereof. An integrated porous material prepared through treating an epoxy resin as a base material, diethylenetriamine as a curing agent and polyethylene glycol as a pore forming agent and utilizing an in-situ gradual polymerization process is adopted as a solid phase micro-extraction material, the form of the solid phase micro-extraction material to prepare a solid micro-extraction column is combined with a rotation-speed-adjustable motor, a stirring effect is realized through rotation, and simultaneously the solid phase micro-extraction material which is adopted as an electrical adsorption work electrode and a platinum wire electrode which is adopted as a counter electrode are combined with a high-voltage direct current power supply to realize an electric adsorption effect in order to complete the electrically-driven solid phase micro-extraction. The electrically-driven solid phase micro-extraction method combining the electric adsorption technology with the stirring technology effectively overcomes a disadvantage that magnetic stirring cannot be used in a small-volume solution and simultaneously reduces a disadvantage that the abrasion of a solid phase micro-extraction stirring bar is easy, so the service life can be prolonged; the integrated epoxy resin based porous polymer is treated as the adsorption material, so the extraction amount and the detection sensitivity are improved. The method has the advantages of simplicity, easy operation and high flexibility.

Description

Technical field [0001] The invention relates to an electric-driven accelerated solid-phase micro-extraction method and a device thereof. It is a pre-enrichment separation technology for multiple analysis methods and belongs to the laboratory application category. Background technique [0002] Solid-phase micro-extraction (SPME), which integrates sampling, extraction, enrichment, separation, and injection, has become one of the important sample pretreatment techniques. It is different from conventional solid-phase extraction (Solid-phase Compared with extraction (SPE) technology, the sample pretreatment time can be significantly shortened, thereby improving analysis efficiency. For example, a complete SPE process often takes 30-60 minutes, while the SPME process can be reduced to 10-30 minutes. However, when faced with a large-scale sample analysis task, especially compared to a large-scale instrument measurement process that can be completed within minutes or even seconds, it is...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/34G01N1/40
Inventor 王邃陶艳玲邓爱妮危晶郭帧张宁郭智勇陆其红
Owner NINGBO UNIV
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