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Preparation method for solid-phase micro-extraction fiber bundle

A technology for extracting fibers and fibers, which is applied in the field of preparation of solid-phase microextraction fiber bundles, can solve the problems of prolonging the adsorption and analysis time, affecting the service life, reducing the mass transfer speed, etc., achieving high extraction capacity, improving extraction speed, and method easy effect

Inactive Publication Date: 2014-06-18
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to increase the extraction capacity, it is necessary to increase the thickness of the extraction medium (coating), but the increase in the thickness of the coating will lead to a decrease in the mass transfer rate, thereby prolonging the adsorption and desorption time; in addition, too thick coating is easy to crack and affect the service life

Method used

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  • Preparation method for solid-phase micro-extraction fiber bundle
  • Preparation method for solid-phase micro-extraction fiber bundle
  • Preparation method for solid-phase micro-extraction fiber bundle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Preparation of a single SPME fiber based on the overall material: the monomer mixture (containing 20% ​​octadecyl methacrylate, 79.5% divinylbenzene and 0.5% azobisisobutyronitrile) and The porogen (containing n-propanol and cyclohexanol, with a mass percentage of 30% / 70%) was mixed at 30% / 70% to form a uniform solution, and then injected into a quartz crystal with a length of 5cm, an inner diameter of 0.2mm, and a wall thickness of 0.05mm. In the capillary, both ends were sealed, and polymerized at 50°C for 6h. After the polymerization, the 1cm capillary was removed, and the whole material fiber was placed in a Soxhlet extractor, and acetonitrile was used as a solvent for extraction for 4 hours.

[0020] 2) Preparation of SPME fiber bundles: Take 2 fibers prepared in step 1), and bind the 2 fibers together with a sealing film in the capillary part to obtain SPME fiber bundles.

Embodiment 2

[0022] 1) Preparation of a single SPME fiber based on the overall material: the monomer mixture (containing 60% vinylpyridine, 39% divinylbenzene and 1.0% benzoyl peroxide) and porogen (containing positive propanol and 1,4-butanediol (mass percentage is 50% / 50%) mixed at 40% / 60% to form a uniform solution, and then injected into a quartz capillary with a length of 10cm, an inner diameter of 0.4mm, and a wall thickness of 0.05mm , Sealed at both ends, polymerized at 60°C for 12h. After the polymerization, the 1.5 cm capillary was removed, and the whole material fiber was placed in a Soxhlet extractor, and methanol was used as a solvent for extraction for 8 hours.

[0023] 2) Preparation of SPME fiber bundles: take 3 fibers prepared in step 1), and bind the 3 fibers together with adhesive tape in the capillary part to obtain SPME fiber bundles.

Embodiment 3

[0025] 1) Preparation of a single SPME fiber based on the overall material: the monomer mixture (containing 35% vinylimidazole, 63% divinylbenzene and 2.0% azobisisobutyronitrile) and porogen (containing n-propanol and 1,4-butanediol (60% / 40% by mass) were mixed into a uniform solution at 60% / 40%, and then injected into a glass tube with a length of 10cm, an inner diameter of 0.5mm, and a wall thickness of 0.1mm In the process, both ends were sealed and polymerized at 70°C for 12h. After the polymerization, the 2cm capillary was removed, and the whole material fiber was placed in a methanol solvent, soaked until no impurities were detected in the liquid. figure 1 It is a physical picture of a single SPME fiber of the overall material.

[0026] 2) Step 2: Preparation of SPME fiber bundles: Take 4 fibers prepared in step 1), and combine the 4 fibers with raw material tape in the capillary part to obtain SPME fiber bundles. figure 1 Schematic diagram of the SPME fiber bundle co...

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Abstract

The invention relates to a preparation method for a solid-phase micro-extraction fiber bundle, and relates to preparation of the fiber bundle. The preparation method comprises the steps of (1) preparation of single SPME (solid-phase micro-extraction) fibers based on an integral material: mixing a monomer, a crosslinking agent, a pore-forming agent and an initiator to prepare a uniform solution, then injecting the uniform solution into a capillary which is 5-20cm long and of which the inner diameter is 0.2-0.8mm and the wall thickness is 0.05-0.2mm, sealing two ends of the capillary, performing polymerization, removing a section, which is 1-3cm long, of the capillary, putting the integral material fiber into a soxhlet extractor, performing extraction through a solvent, or putting the fiber into the solvent, and soaking the fiber until no impurity is detected from the liquid so as to obtain the single SPME fibers based on the integral material; (2) preparation of the solid-phase micro-extraction fiber bundle: combining 2-6 of the single SPME fibers based on the integral material on the capillary to obtain the solid-phase micro-extraction fiber bundle. The preparation method is simple, high in extraction capacity, high in extraction speed, low in cost and easy to operate.

Description

technical field [0001] The invention relates to a preparation of fiber bundles, in particular to a preparation method of solid phase microextraction fiber bundles. Background technique [0002] The solid-phase microextraction (SPME) technique was proposed by Pawliszyn et al. (Anal.Chem., 1990, 62:2145-2148) in Canada in 1990. This technology is developed on the basis of solid phase extraction. The usual practice is to apply the extraction medium on the surface of quartz fiber or other materials similar to the shape of quartz fiber, and then insert the fiber into the sample solution. The extraction equilibrium is reached between the solution and the extraction medium (this process can also be carried out in the way of headspace). After the extraction, the target substance is resolved from the fiber extraction medium by thermal analysis or solvent analysis. Solid-phase microextraction retains most of the advantages of solid-phase extraction (SPE), and overcomes some shortcomi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30B01J20/26B01J20/28C08F212/36C08F226/06C08F220/18C08J9/28
Inventor 黄晓佳梅蒙张咏袁东星
Owner XIAMEN UNIV
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