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Rapid separation and detection method of vinyl triazole product

A vinyl triazole and detection method technology, applied in the direction of material separation, measuring devices, and analysis materials, etc., can solve the problems of difficult sample recovery, low precision of gas chromatography, poor safety, etc.

Active Publication Date: 2017-03-15
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] For this reason, the technical problem to be solved by the present invention is that existing gas chromatographic precision is low, safety is poor, and sample is not easy to reclaim, and there is not a kind of high performance liquid chromatographic separation of vinyltriazole product in existing reports. method, and then proposed a rapid separation and detection method for vinyl triazole products. The chromatographic column was prepared with porous polyglycidyl methacrylate microspheres modified by diazo resin, and the vinyl triazole was detected by HPLC. Rapid Separation of Azole Products

Method used

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  • Rapid separation and detection method of vinyl triazole product
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  • Rapid separation and detection method of vinyl triazole product

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preparation example Construction

[0032]The preparation method of the vinyl triazole product in the embodiment 1-5 is: the vinyl triazole product obtained by the elimination reaction of triazole and vinyl acetate is obtained after vacuum distillation, extraction, distillation and concentration, specifically For: 150ml (1.62mol) of vinyl acetate, 0.2g of hydroquinone, 9.5g of mercury acetate, 9.6ml of trifluoroacetic acid, 37.0g (0.51mol) of 1,2,4-triazole Add it to a 500ml flask connected with a spherical condenser, and add a magnet to it, stir it vigorously under normal temperature for 10-20min, heat it in an oil bath, and control the reaction temperature to 70°C. The reaction was carried out under the protection of nitrogen. After reacting for 3 hours, stop heating and stirring, and let it stand for cooling. At this time, the solution was dark brown. The solution in the flask was distilled under reduced pressure, and the unreacted vinyl acetate was evaporated under reduced pressure. The remaining liquid in ...

Embodiment 1

[0035] A rapid separation and detection method of a vinyltriazole product in this embodiment comprises the following steps:

[0036] S1. Take 40 microliters of the product and mix it into 3ml of a mixture of acetonitrile and water with a volume ratio of 70:30 to obtain a sample solution to be tested;

[0037] S2, HPLC separation and detection: Disperse 1.25 g of porous polyglycidyl methacrylate microspheres modified by diazo resin in 20 ml of isopropanol, and use a mixture of methanol and isopropanol with a volume of 1:1 as The pressurized liquid was packed into a stainless steel chromatographic column with a height of 75mm and a diameter of 4.6mm by a column packing machine, and the vinyltriazole product sample was separated from the liquid to be tested at a flow rate of 0.5ml / min. Such as Figure 4 As shown, the curve a is the separation effect of the porous microspheres modified by the diazo resin prepared in this example on the vinyl triazole product, and the results show...

Embodiment 2

[0047] A rapid separation and detection method of a vinyltriazole product in this embodiment comprises the following steps:

[0048] S1. Take 50 microliters of the product and mix it into 3.5ml of the mixed solution of acetonitrile and water with a volume ratio of 65:35 to obtain the sample solution to be tested;

[0049] S2. HPLC separation and detection: Disperse 1.40 g of porous polyglycidyl methacrylate microspheres modified by diazo resin in 20 ml of isopropanol, and add a mixture of methanol and isopropanol with a volume of 0.9:1.1. Pressure liquid, packed into a stainless steel chromatographic column with a height of 75 mm and a diameter of 4.6 mm by a column packing machine, with a mixture of acetonitrile and water at a volume ratio of 65:35 as the mobile phase, at a temperature of 25 ° C, the flow rate is 0.6ml / min, the vinyltriazole product sample liquid to be tested was separated by high performance liquid chromatography, showing a good separation effect.

[0050] ...

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Abstract

The invention relates to a rapid separation and detection method of a vinyl triazole product. The method comprises that diazoresin modified porous poly(glyceryl methacrylate) microspheres are used as a filler of a high performance liquid chromatography column; the filler is prepared by the steps of taking uniform-particle-size porous poly(glyceryl methacrylate) microspheres prepared by a multi-step swelling method as a basis, then hydrolyzing the polymer microspheres to obtain hydroxyl, and carrying out optical crosslinking reaction with diazoresin having diazonium groups. Due to the hydrophobicity of the chromatographic column filler, the overall retention time on the vinyl triazole product having hydrophobicity is reduced, and the retention time of a by-product acetic acid is enhanced with use of a secondary amino group of the modified diazoresin, so that the vinyl triazole and the by-product are separated. The method is used for separation and detection of the vinyl triazole product, has the advantages of rapid separation and detection, simple operation and good reproducibility, provides an effective separation means for triazole vinyl, and has relatively high practical value.

Description

technical field [0001] The present invention relates to a compound separation and detection method, in particular to a rapid separation and detection method for vinyl triazole products, to be precise, the porous polyglycidyl methacrylate microspheres prepared by a multi-step swelling method are combined with heavy Nitrogen resin was photocrosslinked to prepare porous polyglycidyl methacrylate microspheres modified by diazo resin, which were used as chromatographic column packing, and high performance liquid chromatography (HPLC) was used to make vinyl triazole and by-products in the separated in a short period of time. Background technique [0002] Vinyltriazole, as a water-soluble compound with carbon-carbon double bond, can obtain a polymer with nitrogen-rich heterocyclic ring through polymerization reaction. The physical and chemical properties of the polymer have attracted widespread attention and have great potential to be applied in ionic liquids, fuel cells, organic ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/60
CPCG01N30/02G01N30/06G01N30/6052
Inventor 于冰丛海林张宏博
Owner QINGDAO UNIV
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