CN102872165A - Production process for efficiently preparing high-content steopractic general flavone - Google Patents

Abstract

The production process adopts 50oC ultrasonic to extract and press gruffs, ceramic membrane micro porous filtration, fine PIPO-00 polystyrene macroporous resin to absorb unsymmetrical high-pressure chromatography, effectively adjusts the ratio of the drug quantity of rhizoma drynariae to drug quantity absorbed by separation material PIPO-00 polystyrene macroporous resin, adopts a multiplecolumn method to balance the reduced capability of resin adsorption, and adopts inverse elution and other technical schemes, solves problems of long production cycle, large fluctuation of general flavone transfer ratio and general flavone content and the like, can control a production cycle to be accomplished within 8 hours, control the general flavone transfer ratio to be about 70 percent, the general flavone content to be 50 to 60 percent, and achieves the technical requirement that the content of the fifth type active ingredient of new traditional Chinese drugs is larger than 50 percent.

Description

A kind of efficient preparation high-load Process of Total Flavonoids in Drynaria Fortunei production technology

Technical field

Patent of the present invention relates to a kind of efficient preparation high-load Process of Total Flavonoids in Drynaria Fortunei production technology, Chinese medicine Rhizoma Drynariae extraction separation and purification field.Ultrasonic extraction, dregs pressing, macroporous adsorbent resin PIPO-00 separation and purification have been adopted, and the advanced asymmetric chromatography theory of employing, the high pressure chromatography, reasonable distribution Rhizoma Drynariae medical material and parting material ratio, adopt the flexible using method of multicolumn, reach two important indicators of the high yield of total flavones and high-load, reduce cost and the specification requirement that reaches national Chinese medicine the 5th kind new medicine 50% above effective ingredient.

Background technology

Compendium of Material Medica: " Rhizoma Drynariae can be controlled tooth to the marrow, and chronic diarrhea dysentery.There is the chronic diarrhea Wei former times, and all doctors are not imitated, and is vertical dangerous, gives and uses this medicamental pulverata, enters to simmer ripe and food in the Ren sus domestica, pauses and.Lid kidney master defecation, chronic diarrhea belongs to suffers from a deficiency of the kidney, can not be specially from taste also ".Modern study finds that Process of Total Flavonoids in Drynaria Fortunei has the curative effect for the treatment of osteoporosis, is used for women's osteoporosis, successful.The commercial production Process of Total Flavonoids in Drynaria Fortunei adopts boiling water extraction, normal pressure Flavonoids by Macroporous Adsorption Resin, the weakness such as it is large that extraction efficiency is low, the production cycle is long, the total flavones rate of transform is low, general flavone content fluctuates.Patent of the present invention adopts 50 ^oThe C ultrasonic extraction, the squeezing medicinal residues, the ceramic membrane microporous filter, the asymmetric high pressure chromatography of meticulous PIPO-00 polystyrene macroporous resin adsorption, effectively having allocated Rhizoma Drynariae medical material amount descends with the ratio row of parting material PIPO-00 macroporous resin adsorption with multicolumn method balance resin absorbability, and the multiple technologies scheme such as anti-phase eluting, the problems such as production cycle length, the total flavones rate of transform and general flavone content fluctuation are large have been solved, the new technology scheme can be finished a production cycle being controlled at 8 hours, the total flavones rate of transform is about 70%, and general flavone content is at 50%-60%.

Summary of the invention

Patent adopts 50 ^oThe C ultrasonic extraction, the squeezing medicinal residues, the ceramic membrane microporous filter, the asymmetric high pressure chromatography of meticulous PIPO-00 polystyrene macroporous resin adsorption, effectively having allocated Rhizoma Drynariae medical material amount descends with the ratio row of parting material PIPO-00 macroporous resin adsorption with multicolumn method balance resin absorbability, and the multiple technologies scheme such as anti-phase eluting, the problems such as production cycle length, the total flavones rate of transform and general flavone content fluctuation are large have been solved, the new technology scheme can be finished a production cycle being controlled at 8 hours, the total flavones rate of transform is about 70%, and general flavone content is at 50%-60%.Reach new Chinese medicine the 5th effective constituents content greater than 50% specification requirement.

1. the Chinese medicine Rhizoma Drynariae 50 ^oUltrasound wave water extraction in the C;

Use first the water of 10 times of weight of Chinese medicine Rhizoma Drynariae and Folium Camelliae sinensis 50 ^oUltrasound wave water extraction in the C filters, and obtains for the first time aqueous extract, merges same 2 times extracting solution again, obtains aqueous extract.

2. dregs pressing goes out to remain medicinal liquid;

Medicinal residues are squeezed out remaining medicinal liquid with squeezer, and merge with aqueous extract in 1, obtain the water extraction amalgamation liquid.

3. ceramic membrane microporous filter;

Hydration becomes complete supernatant liquid with the purpose ceramic-film filter of liquid by the 0.2-0.5 micron pore size.

4. non-linear chromatography loading;

Suitable ratio is PIPO-00: Rhizoma Drynariae medical material 1:4 is to 1:5, loading, and with 5-8 column volume (BV) water pressurization eluting.

5. anti-phase eluting;

With the anti-phase eluting of 4-5BV75% ethanol, collect eluent, the pressurization Recycled ethanol obtains total flavones stream clear paste.

6. microwave drying;

Microwave drying total flavones stream clear paste obtains solid, and crushing screening obtains meticulous Process of Total Flavonoids in Drynaria Fortunei fine powder, can be used for solid preparation.

7. the online anti-phase activating and regenerating method of post;

With the efficient pump of acid and alkali-resistance, use respectively the PIPO-00 parting material in the anti-phase activation post of 5BV-8BV5% sodium hydrate aqueous solution, 5% aqueous hydrochloric acid solution and water 3-5 column volume.

8. balance PIPO-00 absorbability decline solution;

Adopt 6 PIPO-00 detached column methods, each order of classes or grades at school is with 3 PIPO-00 posts, allows the PIPO-00 of 3 posts: Rhizoma Drynariae medical material ratio is 4-5., can obtain general flavone content 50%-60%.When the absorbability of PIPO-00 drop to original absorbability 75% the time, a post of each multiplex the other side's order of classes or grades at school of each order of classes or grades at school, when absorbability drops to 60%, use 5 posts, when absorbability drops to 50%, use 6 posts, can use the whole process of computer record management, guarantee that 2 order of classes or grades at school work are orderly, basically allow PIPO-00: Rhizoma Drynariae medical material ratio remains 4-5., can obtain general flavone content 50%-60%, overcome the general flavone content fluctuation problem.

9. product and process characteristic.

8 hours production cycles, the total flavones rate of transform about 70%, general flavone content 50-60% meets new Chinese medicine the 5th effective constituents greater than 50% specification requirement.

Description of drawings

(not having)

The specific embodiment

Embodiment one:

1. the Chinese medicine Rhizoma Drynariae 50 ^oUltrasound wave water extraction in the C;

Use first the water of 1000 kilograms of Chinese medicine Rhizoma Drynariae 10000 weight and Chinese medicine osteomiosis 50 ^oUltrasound wave water extraction in the C filters, and obtains for the first time aqueous extract, merges same 2 times extracting solution again, obtains aqueous extract.

2. dregs pressing goes out to remain medicinal liquid;

Medicinal residues are squeezed out remaining medicinal liquid with squeezer, and merge with aqueous extract in 1, obtain the water extraction amalgamation liquid.

3. ceramic membrane microporous filter;

Hydration becomes complete supernatant liquid with the purpose ceramic-film filter of liquid by the 0.2-0.5 micron pore size.

10. non-linear chromatography loading;

Suitable ratio is PIPO-00: Rhizoma Drynariae medical material 1:4 namely uses 6 74LPIPO-00 posts to 1:5, and 2 each order of classes or grades at school of order of classes or grades at school use respectively first 3 74LPOPI-00 high-pressure columns, the amalgamation liquid loading, and every post is with 370 kilograms of-592 kg water pressurization eluting.

11. anti-phase eluting;

Every post is collected eluent with 296 kilograms-370 kilograms the anti-phase eluting of 75% ethanol, and the pressurization Recycled ethanol obtains total flavones stream clear paste.

12. microwave drying;

Microwave drying total flavones stream clear paste obtains solid, and crushing screening obtains meticulous Process of Total Flavonoids in Drynaria Fortunei fine powder, can be used for solid preparation.

13. the online anti-phase activating and regenerating method of post;

With the efficient pump of acid and alkali-resistance, use respectively the PIPO-00 parting material in the anti-phase activation post of 5BV-8BV5% sodium hydrate aqueous solution, 5% aqueous hydrochloric acid solution and water 3-5 column volume.

14. balance PIPO-00 absorbability decline solution;

Adopt 6 PIPO-00 detached column methods, each order of classes or grades at school is with 3 PIPO-00 posts, allows the PIPO-00 of 3 posts: Rhizoma Drynariae medical material ratio is 1:4: to 1:5., can obtain general flavone content 50%-60%.When the absorbability of PIPO-00 drop to original absorbability 75% the time, a post of each multiplex the other side's order of classes or grades at school of each order of classes or grades at school, when absorbability drops to 60%, use 5 posts, when absorbability drops to 50%, use 6 posts, can use the whole process of computer record management, guarantee that 2 order of classes or grades at school work are orderly, basically allow PIPO-00: Rhizoma Drynariae medical material ratio remains 1:4: to 1:5., can obtain general flavone content 50%-60%, overcome the general flavone content fluctuation problem.

15. product and process characteristic.

8 hours production cycles, the total flavones rate of transform about 70%, general flavone content 50-60% meets new Chinese medicine the 5th effective constituents greater than 50% specification requirement.

Claims (1)

1. an efficient preparation high-load Process of Total Flavonoids in Drynaria Fortunei production technology is characterized in that comprising the steps:

(1) ultrasound wave water extraction in 50 ℃ of the Chinese medicine Rhizoma Drynariae;

Use first water and Folium Camelliae sinensis ultrasound wave water extraction in 50 ℃ of 10 times of weight of Chinese medicine Rhizoma Drynariae, filter, obtain for the first time aqueous extract, merge again same 2 times extracting solution, obtain aqueous extract;

(2) dregs pressing goes out to remain medicinal liquid;

Medicinal residues are squeezed out remaining medicinal liquid with squeezer, and merge with aqueous extract in 1, obtain the water extraction amalgamation liquid;

(3) ceramic membrane microporous filter;

Hydration becomes complete supernatant liquid with the purpose ceramic-film filter of liquid by the 0.2-0.5 micron pore size;

(4) non-linear chromatography loading;

Suitable ratio is PIPO-00: Rhizoma Drynariae medical material 1:4 is to 1:5, loading, and with 5-8 column volume (BV) water pressurization eluting;

(5) anti-phase eluting;

With the anti-phase eluting of 4-5BV75% ethanol, collect eluent, the pressurization Recycled ethanol obtains total flavones stream clear paste;

(6) microwave drying;

Microwave drying total flavones stream clear paste obtains solid, and crushing screening obtains meticulous Process of Total Flavonoids in Drynaria Fortunei fine powder, can be used for solid preparation;

(7) the online anti-phase activating and regenerating method of post;

With the efficient pump of acid and alkali-resistance, use respectively the PIPO-00 parting material in the anti-phase activation post of 5BV-8BV5% sodium hydrate aqueous solution, 5% aqueous hydrochloric acid solution and water 3-5 column volume;

(8) balance PIPO-00 absorbability decline solution;

Adopt 6 PIPO-00 detached column methods, each order of classes or grades at school is with 3 PIPO-00 posts, allows the PIPO-00 of 3 posts: Rhizoma Drynariae medical material ratio is 4-5., can obtain general flavone content 50%-60%; When the absorbability of PIPO-00 drop to original absorbability 75% the time, a post of each multiplex the other side's order of classes or grades at school of each order of classes or grades at school, when absorbability drops to 60%, use 5 posts, when absorbability drops to 50%, use 6 posts, can use the whole process of computer record management, guarantee that 2 order of classes or grades at school work are orderly, basically allow PIPO-00: Rhizoma Drynariae medical material ratio remains 4-5., can obtain general flavone content 50%-60%, overcome the general flavone content fluctuation problem;

(9) product and process characteristic.

8 hours production cycles, the total flavones rate of transform about 70%, general flavone content 50-60% meets new Chinese medicine the 5th effective constituents greater than 50% specification requirement.