Simulated moving bed splitting method for schisandrin b

A technology of simulated moving bed and schisandrin B, which is applied in the field of simulated moving bed chromatographic separation of schisandrin B, can solve the problems of low efficiency, easy pollution, easy loss, etc., and achieve the effect of simple process and stable product quality

Inactive Publication Date: 2014-01-22
江苏汉邦科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Schisandra chinensis (Turcz.) Baill is a perennial woody vine of Magnoliaceae. The fruit is used as medicine, and the roots and stems can also be used as medicine. , Indications for cough and asthma, thirst, spontaneous sweating, nocturnal emission, chronic diarrhea, neurasthenia, modern research has proved that it also has the functions of regulating blood pressure, protecting the liver and "adaptogen", it is an authentic northern precious medicinal material, Schisandrin B is the main activ

Method used

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  • Simulated moving bed splitting method for schisandrin b
  • Simulated moving bed splitting method for schisandrin b

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Experimental program
Comparison scheme
Effect test

Example Embodiment

[0026] Implementation:

[0027] 1. Preparation of cellulose-tris(3,5-dimethylphenylcarbamate) filler

[0028] Prepared according to the method of literature (Okamoto Y, Kawashima M, Hatada K J. Chromatogr. 1986, 363: 173~186); cellulose and phenyl isohydrogenate were reacted in pyrrole solution at 100 ° C for 24 hours, and the methanol obtained by the reaction The incompatible substance is cellulose-tris(3,5-dimethylphenylcarbamate). Cellulose-tris(3,5-dimethylphenylcarbamate) was dissolved in tetrahydrofuran, and aminopropyl silica gel was added to the solution, and stirred electromagnetically until the tetrahydrofuran was evaporated. Repeat 3 times to obtain cellulose- Tris(3,5-dimethylphenylcarbamate)-coated chiral stationary phase. Wherein the weight ratio of cellulose-tris(3,5-dimethylphenyl carbamate) and aminopropyl silica gel is 1:5;

[0029] 2. Selection of mobile phase flow rate

[0030] The flow rate of the mobile phase affects the separation of the enantiomers ...

Example Embodiment

[0050] Detached instance 1:

[0051] A operating condition

[0052] Mobile phase: methanol

[0053] Injection concentration: 5g / ml

[0054] Injection flow rate: 1.5 ml / min

[0055] Eluent flow rate: 3.0 ml / min

[0056] Extraction flow rate: 2.5 ml / min

[0057] Raffinate flow rate: 2.0 ml / min

[0058] Switching time: 6.8min

[0059] System temperature: 30℃

[0060] B finished product analysis

[0061] The composition of the extract and the raffinate was analyzed with an analytical column. The purity of the extract was 99.9%, and the purity of the raffinate was 99.9%. Each kilogram of stationary phase can produce 23.5kg of R-schisandrin B and S-schisandrin B per day. , the mobile phase consumption is 0.128L / kg, and the recovery rate is 99.2%

Example Embodiment

[0062] Detached instance 2:

[0063] A operating condition

[0064] Mobile phase: methanol

[0065] Injection concentration: 5g / ml

[0066] Injection flow rate: 1.0 ml / min

[0067] Eluent flow rate: 2.5 ml / min

[0068] Extraction flow rate: 1.7 ml / min

[0069] Raffinate flow rate: 1.8 ml / min

[0070] Switching time: 7.5min

[0071] System temperature: 30℃

[0072] B finished product analysis

[0073] The composition of the extract and the raffinate was analyzed with an analytical column. The purity of the extract was 98.2%, and the purity of the raffinate was 98.9%. Each kilogram of stationary phase could produce 18kg of R-schisandrin B and S-schisandrin B per day. The mobile phase consumption was 0.163 L / kg, and the recovery was 97.2%.

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Abstract

The invention discloses a simulated moving bed splitting method for schisandrin b. The method is characterized in that a simulated moving bed chromatographic system is adopted, cellulose-tri (3,5-dimethyl phenyl carbamate) is taken as a filler, and methyl alcohol is taken as a moving phase. High-purity R-schisandrin b and high-purity S-schisandrin b are split from raceme of schisandrin b. The simulated moving bed chromatographic system can realize continuous production and is high in automation degree and production efficiency.

Description

technical field [0001] The invention relates to a separation technology of chiral drugs, in particular to a simulated moving bed chromatographic separation method of schisandrin B. Background technique [0002] Schisandra chinensis (Turcz.) Baill is a perennial woody vine of Magnoliaceae. The fruit is used as medicine, and the roots and stems can also be used as medicine. , Indications for cough and asthma, thirst, spontaneous sweating, nocturnal emission, chronic diarrhea, neurasthenia, modern research has proved that it also has the functions of regulating blood pressure, protecting the liver and "adaptogen", it is an authentic northern precious medicinal material, Schisandrin B is the main active ingredient of Schisandra chinensis, and its content is often used as a quality control indicator in products with Schisandra chinensis as the main raw material. It is also a symbolic component of the fingerprints of Schisandra chinensis and its products. The amount is large, and...

Claims

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Application Information

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IPC IPC(8): C07D317/70
CPCC07D317/70
Inventor 张大兵罗军侠张宁李胜迎王亚辉
Owner 江苏汉邦科技股份有限公司
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