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
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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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