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Gold nanoparticle-polysaccharide bonded silica gel fixed phase and preparation method thereof

A technology of gold nanoparticles and bonded silica gel, applied in the field of materials, can solve the problems of decreased column efficiency, weak ability to separate complex polar compounds, etc., and achieve the effects of reduced detection cost, good selectivity and separation ability, and novel structure

Inactive Publication Date: 2014-09-10
镇江出入境检验检疫局检验检疫综合技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The general stationary phase, such as C18, after using rich water mobile phase for a long time, the column efficiency will be seriously reduced, especially when there are exposed silanol groups, and the ability to separate complex polar compounds is weak

Method used

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  • Gold nanoparticle-polysaccharide bonded silica gel fixed phase and preparation method thereof
  • Gold nanoparticle-polysaccharide bonded silica gel fixed phase and preparation method thereof
  • Gold nanoparticle-polysaccharide bonded silica gel fixed phase and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1).Introduction of chlorinated hydrocarbon functional groups on the surface of silica gel

[0045] Silica gel is spherical silica gel, with a diameter of 5 μm, a pore size of 10 nm, and a specific surface area of ​​380 m 2 / g. Disperse 3 g of pretreated silica gel in 100 mL of anhydrous toluene, add 3 mL of 3-chloropropyltrimethoxysilane, under nitrogen protection, reflux and stir for 24 hours, then filter with a sand core funnel, and use dichloromethane and acetone in sequence , washed with methanol, and finally dried in a vacuum oven at 60° C. for 24 hours to obtain chlorohydrocarbyl-modified silica gel.

[0046] 2). Preparation of polysaccharide-bonded silica gel

[0047] Disperse 3g of silica gel modified with chlorinated hydrocarbon groups in 150mL of anhydrous N,N-dimethylformamide, then add 3g of bitter gourd polysaccharide, and react at 60°C for 20 hours under nitrogen protection; then filter with a sand core funnel, and use Wash with ultra-pure water and met...

Embodiment 2

[0056] Using the gold nanoparticle-polysaccharide bonded silica gel stationary phase obtained in Example 1, the homogenate method is used to fill in a stainless steel column with a length of 150 mm and an internal diameter of 4.6 mm, and the resulting chromatographic column is used for analyzing and separating samples. In phase chromatography mode, five sulfonamide antibiotics were separated: sulfamethoxine, sulfamethazine, sulfamethoxypyridazine, sulfamethazine, sulfadiazine;

[0057] Chromatographic conditions: The mobile phase is a mixture obtained by mixing acetonitrile and 7mmol / L ammonium acetate aqueous solution at a volume ratio of 4:96; the flow rate is 1mL / min; the temperature is room temperature; the detection wavelength is 270nm.

[0058] figure 1 Its chromatographic separation results.

Embodiment 3

[0060] Using the gold nanoparticle-polysaccharide bonded silica gel stationary phase obtained in Example 1, the homogenate method is used to fill in a stainless steel column with a length of 150 mm and an internal diameter of 4.6 mm, and the resulting chromatographic column is used for analyzing and separating samples. In phase chromatography mode, six water-soluble nitrogen-containing compounds are separated: pantothenic acid, ammeline, nicotinic acid, ammeline, melamine, riboflavin;

[0061] Chromatographic conditions: mobile phase is a mixture of acetonitrile and aqueous solution at a volume ratio of 2:98; flow rate is 1mL / min; temperature is room temperature; detection wavelength: 260nm.

[0062] figure 2 Its chromatographic separation results.

[0063] figure 1 with figure 2 It shows that the gold nanoparticle-polysaccharide bonded silica gel stationary phase provided by the present invention has good retention and separation selectivity for polar food additives and ...

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Abstract

The invention discloses a gold nanoparticle-polysaccharide bonded silica gel fixed phase and a preparation method thereof. A structural general formula of the gold nanoparticle-polysaccharide bonded silica gel fixed phase is shown as a formula I. The preparation method comprises the following steps: introducing a chloro-hydrocarbonyl functional group on the surface of silica gel; bonding natural bitter gourd polysaccharide on the surface of the silica gel; fixing carboxylation gold nanoparticles in natural bitter gourd polysaccharide molecules in the presence of the catalysis of 4-dimethylaminopyridine and 1-ethyl-(3-dimethylamino propyl) carbodiimide hydrochloride to obtain the gold nanoparticle-polysaccharide bonded silica gel fixed phase. The preparation process is simple, the fixed phase is novel in structure, stable in property and flexible in application; polar food additives and illegal additives are well retained and separately selected in a water-rich chromatographic mode. Meanwhile, according to the water-rich mode, ultrapure water serves as a mobile phase mainly, so that pollution caused by adoption of an organic solvent as the mobile phase in the prior art is avoided, a large number of solvents are saved, and the detection cost is reduced.

Description

technical field [0001] The invention belongs to the field of materials, and relates to a preparation method of a liquid chromatography stationary phase, in particular to a gold nanoparticle-polysaccharide bonded silica gel stationary phase and a preparation method thereof. Background technique [0002] Food additives are widely used in food production and are an important part of the modern food industry. According to national regulations, there are only more than 2,000 kinds of additives allowed to be used in food, and some unscrupulous manufacturers lack integrity and add some illegal ingredients to processed foods to increase the color and taste of food or fake main ingredients. For example, the dicyandiamide and melamine incidents in dairy products, the "leather milk" incident, and the incidents of adding sodium copper chlorophyllin to soybean oil as olive oil, etc. The harm caused by the abuse of illegal additives is still talking about discoloration. Whether it is foo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 陈桐李平周洪斌肖震宋广三张慧勤李静
Owner 镇江出入境检验检疫局检验检疫综合技术中心
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