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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AI-Extracted Technical Summary

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...
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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.

Application Domain

Technology Topic

ChemistrySimulated moving bed +7

Image

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

Examples

  • Experimental program(3)

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 of Schisandra B, and also affects the production efficiency of simulated moving bed chromatography. First, a column (10*250mm) of the simulated moving bed chromatography system is used for flow rate selection analysis, see Table 1 ,
[0031] Table 1 Selection of mobile phase flow rate
[0032]
[0033] Simulate the separation of a moving bed
[0034] Mobile phase: methanol
[0035] Injection concentration: 0~100g/ml
[0036] Injection flow rate: 0~50ml/min
[0037] Flow rate of eluent: 0~1000ml/min
[0038] Extraction flow rate: 0~100ml/min
[0039] Participating fluid flow rate: 0~100ml/min
[0040] Switching time: 3~20min
[0041] Column temperature: 0~50℃
[0042] 3. Finished product inspection
[0043] Pump: Jiangsu Hanbang Technology Analysis Pump
[0044] Detector: Jiangsu Hanbang Technology UV Detector
[0045] Detection wavelength: 254nm
[0046] Mobile phase: methanol
[0047] Flow rate: 0.8ml/min
[0048] Chromatographic column: 4.6*250mm packing is self-coated cellulose-tris(3,5-dimethylphenylcarbamate)
[0049] Two examples of separation are listed below:

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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PUM

PropertyMeasurementUnit
Wavelength254.0nm
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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  • Simple process
  • Product quality is stable
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