Oral preparation containing caffeic acid ester and breviscapine and preparation method thereof
A caffeic acid ester and oral preparation technology, which is applied in the application field of preparing anti-tumor drugs, can solve the problems that impurities are easy to solidify, cannot be eluted, and columns are difficult
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Embodiment 1
[0135] Example 1: Preparation of raw material drug extract
[0136] Take 2000 g of Asarum radix and add 50% aqueous ethanol to decoct twice, 2 hours each time, filter, combine the filtrates, and concentrate under reduced pressure to form an extract (relative density 1.15-1.25, 75°C); add 5 times the amount of the extract Add 5% sodium hydroxide solution under stirring to adjust pH 7.5~8.5, filter, add 10% sulfuric acid solution to adjust pH 1~3, leave overnight, filter, collect filtrate and precipitate, precipitate with ethanol, and then Add 5% sodium hydroxide to adjust the pH value to 7-8, spray dry to obtain powder 1; adjust the pH value of the acidified filtrate to 7-9, use a 100nm ceramic membrane for clarification, and use a 350D organic membrane for the clarified solution obtained after clarification. Concentrated, the concentrated solution was passed through a 30-60 mesh polyamide chromatography column (diameter to length ratio of 1:4), eluted with water for 3 column v...
Embodiment 2
[0137] Example 2: Preparation of raw drug extracts
[0138] Take 2000 g of Asarum radix and add 50% aqueous ethanol to decoct twice, 2 hours each time, filter, combine the filtrates, and concentrate under reduced pressure to form an extract (relative density 1.15-1.25, 75°C); add 5 times the amount of the extract Add 5% sodium hydroxide solution under stirring to adjust pH 7.5~8.5, filter, add 10% sulfuric acid solution to adjust pH 1~3, leave overnight, filter, collect filtrate and precipitate, precipitate with ethanol, reduce Press-dried to obtain powder 1; the acidified filtrate was adjusted to pH 7-9, clarified with a 100nm ceramic membrane, the clarified solution obtained after clarification was concentrated with a 350D organic membrane, and the concentrated solution passed through a 30-60 mesh polyamide chromatography column (diameter to length ratio 1:4), after eluting 3 column volumes with water, eluting 4 column volumes with 65% ethanol, collecting the ethanol eluent,...
Embodiment 3
[0139] Example 3: Preparation of raw drug extracts
[0140] Take 3000 g of Asarum radix and add 60% aqueous ethanol to decoct twice, 2 hours each time, filter, combine the filtrates, and concentrate under reduced pressure to form an extract (relative density 1.15-1.25, 75°C); add 5 times the amount of extract Dissolve in water, add 5% sodium hydroxide solution with stirring, adjust pH 7-9, filter, add 10% hydrochloric acid solution to adjust pH 1-3, leave overnight, filter, collect filtrate and precipitate, precipitate with ethanol, add Adjust the pH value to 7-8 with 5% sodium hydroxide, and spray dry to obtain powder 1;
[0141] The acidified filtrate was adjusted to pH 7-9, clarified with a 200nm ceramic membrane, the clarified solution obtained after clarification was concentrated with a 400D organic membrane, and the concentrated solution passed through a 30-60 mesh polyamide chromatography column (diameter to length ratio of 1). : 4), after eluting with 3 column volumes...
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