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Preparation method of tribenoside isomers

A technology of tribenzyl sugar and isomerization, which is applied in the field of preparation of tribenzyl glycoside isomerization monomer, can solve the problems of low purity, long time of tribenzyl glycoside isomerization monomer, etc., and achieves a simplified and easily controllable process technology. Effect

Active Publication Date: 2014-02-19
江苏汉邦科技股份有限公司
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Problems solved by technology

[0003] The object of the present invention is to solve the problems of long time and low purity in the process of preparing tribenzyl glycoside isomers, and to provide a method for preparing high-purity tribenzyl glucoside isomers using a preparative liquid chromatography separation system. A new method for the body, the method includes the following steps:

Method used

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  • Preparation method of tribenoside isomers
  • Preparation method of tribenoside isomers
  • Preparation method of tribenoside isomers

Examples

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Embodiment 1

[0016] 1. Take 50 g of crude tribenzyl glucoside and mix it with n-hexane / ethyl acetate solution with a volume ratio of 4:1, configure it into a saturated solution, put it in a filter device, and filter to remove solid particles;

[0017] 2. Inject the tribenzyl glucoside solution into the preparative liquid phase preparative chromatographic separation system, the dynamic axial compression column size is Φ50×250mm, the silica gel filler is the product of Fuji, Japan, the particle size is 20~45um, the sample volume is 30g, and the mobile phase flow rate It is 80ml / min. At the initial stage of separation, the mobile phase n-hexane / ethyl acetate volume ratio ranged from 98 / 2 to 90 / 10. After elution for 40 minutes, the mobile phase n-hexane / ethyl acetate volume ratio was switched to 80 / 20-70 / 30. When the separation time reaches 65 minutes, switch the mobile phase to pure ethyl acetate, so that the impurities at the back end can be washed out, and a separation cycle ends. The dete...

Embodiment 2

[0019] 1. Take 150g of crude tribenzyl glucoside and mix it with n-hexane / ethyl acetate solution with a volume ratio of 6:1, configure it into a saturated solution, place it in a filter device, and filter to remove solid particles;

[0020] 2. Inject the tribenzyl glucoside solution into the preparative liquid phase preparative chromatographic separation system, the dynamic axial compression column size is Φ100×250mm, the silica gel filler is a product of Fuji, Japan, the particle size is 20~45um, the sample volume is 120g, and the mobile phase flow rate It is 300ml / min. At the initial stage of separation, the mobile phase n-hexane / ethyl acetate volume ratio was 98 / 2~90 / 10, and after 40 minutes of elution, the mobile phase n-hexane / ethyl acetate volume ratio was switched to 85 / 15~70 / 30, and the elution At 65 minutes, the mobile phase was switched to pure ethyl acetate, so that the back-end impurities were washed out, and a separation cycle ended. The detection wavelength of t...

Embodiment 3

[0022] 1. Take 300g of crude tribenzyl glucoside and mix it with n-hexane / ethyl acetate solution with a volume ratio of 8:1, configure it into a saturated solution, place it in a filter device, and filter to remove solid particles;

[0023] 2. Inject the tribenzyl glucoside solution into the preparative liquid phase preparative chromatographic separation system, the dynamic axial compression column size is Φ150×300mm, the silica gel filler is a product of Fuji, Japan, the particle size is 20~45um, the sample volume is 250g, and the mobile phase flow rate It is 650ml / min. At the initial stage of separation, the mobile phase n-hexane / ethyl acetate volume ratio was 98 / 2~90 / 10, and after 40 minutes of elution, the mobile phase n-hexane / ethyl acetate volume ratio was switched to 85 / 15~70 / 30, and the elution At 65 minutes, the mobile phase was switched to pure ethyl acetate, so that the back-end impurities were washed out, and a separation cycle ended. The detection wavelength of t...

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Abstract

The invention discloses a preparation method of tribenoside isomers. A tribenoside synthetic crude product is used as a raw material. A proper mobile phase and proper column separation conditions are optimized by HPLC optimization, and amplified to an industrial preparative liquid chromatogram separating system to obtain two tribenoside optical isomers, namely [alpha] and [belta] tribenoside isomers, with high purity. The method is advantageous in that the synthetic crude product can be directly used in the industrial preparative liquid chromatogram separating system to obtain the [alpha] and [belta] tribenoside isomers and achieve good separation and purification effects; the method has simple operation, short period and high efficiency; the purity can reach over 99.5%; and the content of any individual impurity can be controlled to be lower than 0.2%.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, and in particular relates to a preparation method of a tribenzyl glycoside isomer. Background technique [0002] Tribenoside (TBS), namely ethyl-3,5,6-tribenzyloxy-D-glucofuranoside, consists of two optical isomers (α-ethyl-3,5,6 -tribenzyloxy-D-glucopyranoside) and β-body (β-ethyl-3,5,6-tribenzyloxy-D-glucofuranoside). It has the functions of anti-inflammation, anti-toxin, enhancing the tenacity of capillaries, protecting wounded tissue and promoting its healing, and weak analgesic effect. Combining with sphingosine can prevent Gram-negative and positive bacteria. The drug was discovered and synthesized in the 1950s, and was first developed by Japan in 1999 as an oral drug for the treatment of hemorrhoids. Because it is extremely fat-soluble, easily absorbed by the small intestine, and has a high drug utilization rate, its clinical efficacy is relatively high. Other similar drugs have grea...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/06
Inventor 张大兵张宇王亚辉居延娟沈健增
Owner 江苏汉邦科技股份有限公司
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