Simulated moving bed splitting method for schisandrin b

[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:

[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%

[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%.