Clathrate of paeonol and preparation method and quality detection method thereof
A paeonol and clathrate technology, which is applied in the field of clathrates of active ingredients in traditional Chinese medicine, can solve the problems of long time spent, low yield, unfavorable large-scale industrial production, etc.
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Embodiment 1
[0141] 1. Preparation of paeonol inclusion compound:
[0142] Take β-cyclodextrin of 6 times the amount of paeonol, add 2 times the amount of water and stir well, heat to 55°C; take paeonol and add 4 times the amount of 85% ethanol, heat to dissolve and pour into β-cyclodextrin Grind in the fine solution for 15 minutes with a colloid mill, discharge the material, place it at room temperature for 14 hours, filter it with suction, and dry it at 40°C to obtain paeonol inclusion compound.
[0143] 2. Detection of paeonol inclusion complex
[0144] (1) Chromatographic conditions: gas chromatograph; capillary chromatographic column with 5% diphenyl-95% dimethylsilane copolymer as stationary phase; inlet temperature: 230°C; detector temperature (FID): 240°C ;Split ratio: 25:1; Temperature program: initial temperature 80°C, keep for 2min, increase to 160°C at 20°C per minute, keep for 6min, measure; carrier gas: nitrogen, flow rate: 1.0ml / min; injection: 2μl ; The number of theoreti...
Embodiment 2
[0150] 1. Preparation of paeonol inclusion compound:
[0151] Take β-cyclodextrin of 10 times the amount of paeonol, add 2.7 times the amount of purified water and stir well, heat to 60°C; take paeonol and add 5 times the amount of 95% ethanol, heat to dissolve and pour into β-cyclodextrin Grind in dextrin solution for 20 minutes with a colloid mill, discharge, stand at room temperature for 24 hours, filter with suction, and dry at 50°C to obtain paeonol inclusion compound. Detection of paeonol inclusion complex
[0152] (1) Chromatographic conditions: gas chromatograph; capillary chromatographic column with 5% diphenyl-95% dimethylsilane copolymer as stationary phase; inlet temperature: 220°C; detector temperature (FID): 230°C ;Split ratio: 20:1; Temperature program: initial temperature 80°C, keep for 2min, increase to 160°C at 20°C per minute, keep for 6min, measure; carrier gas: nitrogen, flow rate: 1.0ml / min; injection: 5μl ; The number of theoretical plates is calculat...
Embodiment 3
[0158] 1. Preparation of paeonol inclusion compound:
[0159] Take β-cyclodextrin with 14 times the amount of paeonol, add 4 times the amount of water and stir well, heat to 70°C; take paeonol and add 7 times the amount of 90% ethanol, heat to dissolve and pour into β-cyclodextrin Grind in the fine solution for 30 minutes with a colloid mill, discharge the material, place it at room temperature for 24 hours, filter it with suction, and dry it at 60°C to obtain paeonol inclusion compound.
[0160] 2. Detection of paeonol inclusion complex
[0161] (1) Chromatographic conditions: gas chromatograph; capillary chromatographic column with 5% diphenyl-95% dimethylsilane copolymer as stationary phase; inlet temperature: 240°C; detector temperature (FID): 250°C ;Split ratio: 25:1; Temperature program: initial temperature 80°C, keep 2min, increase to 160°C at 20°C per minute, keep 6min, measure; carrier gas: nitrogen, flow rate: 1.0ml / min; injection: 10μl ; The number of theoretical ...
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