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: 2013-01-16
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
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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.), clean it, and apply a thin layer of commercially available epoxy resin adhesive after drying, and wait until it is completely cured for later use.
[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 2 minutes, cool to room temperature, then add 0.5g diethylenetriamine, and mix thoroughly for 2 minutes Obtain a uniform, transparent viscous liquid, pour it into a 1mL disposable syringe (made of polypropylene, the inner diameter of the tube is about 5mm), inject the liquid with a length of about 10-15mm, and immerse the aforementioned treated stainless steel wire 2 vertically in the reaction In the liquid, leave a section out of the reaction liquid, seal it and place it in an oven at 60°C for 24 hours of reaction, and take the prepared solid-phase microextraction column 3 out of the container.
[00...
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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 microextraction method and a device thereof, which is a pre-enrichment separation technology for various analysis methods and belongs to the laboratory application category. Background technique [0002] Solid-phase micro-extraction (SPME), which integrates sampling, extraction, enrichment, separation, and sample injection, has become one of the important sample pretreatment techniques. Extraction, SPE) technology can significantly shorten the sample pretreatment time, thereby improving the 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 number of sample analysis tasks, especially compared to the large-scale instrumental measurement process that can be completed within minutes or even seconds, it is still of great significance to further shorten the time of SPME...
Claims
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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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