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High pH tolerance chromatographic filler and preparation method thereof

A technology of chromatographic packing and reactivity, which is applied in the field of functional chemical materials and its preparation, can solve the problems of unpredictable separation selectivity, loss of chromatographic performance, low mechanical strength, etc., and achieve weakened tailing effect and reduced silanol group density , the effect of high mechanical strength

Active Publication Date: 2013-06-26
月旭科技(上海)股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this has excellent pH stability (pH1-12), it also brings some disadvantages of the polymer matrix, such as low column efficiency, high column pressure, excessive tailing, unpredictable separation selectivity and low mechanical strength. These shortcomings are at least partly due to the large range of pore size distribution
In fact, only the organic matter contained in the surface layer can resist the erosion of high pH mobile phase. When the mobile phase starts to contact the inner matrix, the chromatographic performance has already been caused by the column bed collapse and adsorption caused by the erosion of the surface layer. The stationary phase of the surface layer is completely or almost completely lost, so the organic hybridization of the inner layer is wasteful and unnecessary

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Dissolve 10 grams of TEOS (concentration 95% tetraethoxy silicon) in 20 ml of n-hexane, and mix with 18 grams of tris (dimethylamino) ethylsilane (tris (dimethylamino) ethylsilane), add 0.2 ml of 5% HCl solution as a catalyst, stirred at room temperature for 10 minutes and then placed for use.

[0028] The second step: 109.5 grams of particles with a particle size of 5um, a pore size of 120 angstroms, and a specific surface area of ​​320m 2 / g of bare silica gel, dried under vacuum at 120 degrees Celsius for more than 2 hours, accurately weighed the dried silica gel to be 100.1 grams; added to a round bottom flask with a capacity of 1 liter; then added 500.5ml of chromatographic grade toluene reagent, mixed with silica gel After stirring and mixing, add all the products of the first step reaction into the round bottom flask, continue to stir and heat to reflux for more than 12 hours.

[0029] Step 3: After cooling, filter and wash the product with toluene, meth...

Embodiment 2

[0033]Step 1: Dissolve 10 grams of TEOS (concentration 95% tetraethoxy silicon) in 20 ml of n-hexane, mix with 22 grams of tris(dimethylamino)ethylsilane, add 0.2 ml of 5% HCl solution for Catalyst, after stirring at room temperature for 10 minutes, place it for use.

[0034] The second step: 110.3 grams of particles with a particle size of 5um, a pore size of 120 angstroms, and a specific surface area of ​​320m 2 / g of bare silica gel, dried under vacuum at 120 degrees Celsius for more than 2 hours, accurately weighed the dried silica gel to be 100.3 grams; added to a round bottom flask with a capacity of 1 liter; then added 501.5ml of chromatographic grade toluene reagent, mixed with silica gel After stirring and mixing, add all the products of the first step reaction into the round bottom flask, continue to stir and heat to reflux for more than 12 hours.

[0035] Step 3: After cooling, filter and wash the product with toluene, methanol, hot water and acetone respectively t...

Embodiment 3

[0039] Step 1: Dissolve 10 grams of TEOS (concentration 95% tetraethoxy silicon) in 20 ml of n-hexane, mix with 22 grams of tris(dimethylamino)ethylsilane, add 0.2 ml of 5% HCl solution for Catalyst, after stirring at room temperature for 10 minutes, place it for use.

[0040] The second step: 109.8 grams of particles with a particle size of 5um, a pore size of 120 angstroms, and a specific surface area of ​​320m 2 / g of bare silica gel, vacuum-dry at 120 degrees Celsius for more than 2 hours, accurately weigh the dried silica gel to 100 grams; add it to a round-bottomed flask with a capacity of 1 liter; then add 500ml of chromatographic grade toluene reagent, and stir with the silica gel After mixing, all the products of the first step reaction were added in this round bottom flask, and then 50 g of pyridine was added, and the stirring was continued and heated to reflux for more than 12 hours.

[0041] Step 3: After cooling, filter and wash the product with toluene, methanol...

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Abstract

The invention provides a high pH tolerance chromatographic filler and a preparation method thereof. The filler is prepared by using ultra-pure entire porous spherical silica gel as matrix, and coating a high pH tolerance inorganic / organic hybrid layer with the thickness of several nm through a reaction for surface modification in advance. The filler not only keeps the advantages of other silica-based fillers, but also overcomes the defects of narrow pH range of the traditional silica-based fillers, so as to broaden the PH range to 1-12.5. In the preparation of the filler, an inorganic / organichybrid polymer is prefabricated, then the inorganic / organic hybrid polymer is reacted with the silica gel matrix, and the hybrid layer is coated on the silica gel matrix.

Description

technical field [0001] The invention relates to a functional chemical material and a preparation method thereof, in particular to a high-performance chromatographic filler used for component separation and purification and content analysis and determination in the fields of medicine, food, chemical industry, environmental protection and the like and a preparation method thereof. Background technique [0002] More than 80% of today's small molecule drugs have one or more easily ionizable groups. Compared with the original neutral state, the drug molecules in the ionic state have a large difference in solubility and hydrophobicity. Under ordinary reversed-phase chromatographic conditions (pH2-7), the chromatographic separation effect is very poor. Adjust mobile phase pH to weak base pK a 2 units larger or 2 units smaller than the pKa of the weak acid can effectively inhibit the occurrence of ionization and make most of the drug molecules in a neutral molecular state, thus ach...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/282B01J20/286B01J20/30
Inventor 赵岳星姚立新任兴发夏微微张新华李崟邹乐冰
Owner 月旭科技(上海)股份有限公司
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