Preparation method and mass control method for mahonia duclouxiana gagnep total alkaloids
A method of quality control and a technology of ten ingredients, which is applied in the field of preparation of total alkaloid extracts, can solve problems such as lag in the development and utilization of long column alkaloids, uncontrollable quality, unstable curative effect, etc., and achieve reasonable, stable and feasible process conditions. Addressing deficiencies and multi-indicator charges with high cost and low residue effects
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Embodiment 1
[0037] Take Changzhu Shigonggong and crush it into 500 g of coarse powder, extract with 10 times the amount of 50% ethanol-hydrochloric acid (100:0.5), heat in a water bath at 80 ℃ for 3 times, each time for 2.5 hours, filter, and concentrate the filtrate under reduced pressure No alcohol smell, add water to make up to 5000 ml (0.1 g medicinal materials / ml), filter through four layers of gauze to a clear liquid, filter, pass through an AB-8 macroporous adsorption resin column (the sample liquid is 5 times the volume of the resin), and put on The column flow rate was 1 BV / h. Wash with 2 times of water, discard the washing solution, and elute with 5 times of 20% ethanol at a flow rate of 1 BV / h. Collect the eluent, concentrate the eluent under reduced pressure to the extract, and dry it in vacuum at 60°C to obtain the extract of the total alkaloids of Changzhu Shigong. 59.40%.
Embodiment 2
[0039]Take the long column ten major contributions and crush it into 1 kg of coarse powder, extract with 15 times the amount of 70% ethanol-hydrochloric acid (100:0.5), heat in a water bath at 80°C for 3 times, each time for 1 hour, filter, and concentrate the filtrate under reduced pressure No alcohol smell, add water to make up to 6250 ml (0.16g medicinal materials / ml), filter through four layers of gauze to a clear solution, filter, pass through an AB-8 macroporous adsorption resin column (the sample solution is 6 times the volume of the resin), and put on The column flow rate was 2 BV / h. Wash with 2 times of water, discard the water washing solution, elute with 10 times of 10% ethanol, collect the eluent, and the elution flow rate is 2 BV / h. The eluent was concentrated under reduced pressure to the extract, dried in vacuo at 60°C, and the extract of the total alkaloids of Changzhu Shigong was obtained. The measurement results showed that the content of the three main alkal...
Embodiment 3
[0041] Take the long column and crush it into 1 kg of coarse powder, extract it with 5 times the amount of 90% ethanol-hydrochloric acid (100:0.5), heat it in a water bath at 80°C for 0.5 hours each time, filter it, and concentrate the filtrate under reduced pressure No alcohol smell, add water to make up to 5000 ml (0.2g medicinal material / ml), and the flow rate on the column is 3 BV / h. Filter through four layers of gauze to a clear solution, filter, pass through a D101 macroporous adsorption resin column (the sample solution is 10 times the resin volume), wash with 2 times water, discard the washing solution, and elute with 5 times 30% ethanol, The elution flow rate was 3 BV / h. Collect the eluent, concentrate the eluent under reduced pressure to the extract, and dry it in vacuum at 60°C to obtain the extract of the total alkaloids of the long-column tenaculum. As a result, the contents of the three main alkaloids of the long-column tenagan are: 55.35%.
[0042] The quali...
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