CN102690193A - Preparation technology of tanshinol using spray counterflow extraction method - Google Patents
Preparation technology of tanshinol using spray counterflow extraction method Download PDFInfo
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- CN102690193A CN102690193A CN2012100863098A CN201210086309A CN102690193A CN 102690193 A CN102690193 A CN 102690193A CN 2012100863098 A CN2012100863098 A CN 2012100863098A CN 201210086309 A CN201210086309 A CN 201210086309A CN 102690193 A CN102690193 A CN 102690193A
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Abstract
The invention discloses a preparation technology of tanshinol using a spray counterflow extraction method, and the technology comprises the steps of: removing impurities of medicinal materials of salviae miltiorrhizae, and smashing the materials; decocting the materials in water and extracting the materials 3 times, conducting pressure reduced concentration on filtrate to form liquid extract, adding dilute mineral acid or organic acid to adjust a pH value, carrying out standing to ensure complete settlement of a precipitate, removing solid impurities appearing after acidification by adopting a centrifuge method; and conducting spray counterflow extraction with ethyl acetate, and concentrating and drying the extracted liquid to obtain a finished tanshinol product. The preparation technology of the invention has high extraction efficiency, and benefits to full utilization of traditional Chinese medicine resources; and has the advantages of high medicinal dreg use efficiency reaching 95%, complete extraction, small dosage of solvent, short production cycle, small equipment investment, and low operating cost.
Description
Technical field
The present invention relates to active ingredient of natural plant extraction and separation technology field, particularly a kind of technology of utilizing the spraying counter-current extraction to prepare Salvianic acidA.
Background technology
Salvianic acidA is the main active ingredient of salvia-soluble; Through pharmacological evaluation proof Salvianic acidA is the effective constituent of resisting myocardial ischemia, Salvianic acidA can suppress thrombocyte synthetic, assemble and discharge vaso-excitor material such as TXA2, improve myocardial hypoxia tolerance; The protection cardiac muscle increases coronary flow.These pharmacological actions are the main mechanism of Treated with Radix Salviae Miltiorrhizae coronary heart disease, myocardial ischemia.Therefore, the extraction process of research Salvianic acidA has certain practical significance.Conventional method of extraction is a water extract-alcohol precipitation, and this also is the main process for extracting for preparing Radix Salviae Miltiorrhizae Injection and oral liquid at present.Weak point is that alcohol concn is too high, makes that liposoluble ingredients such as main active ingredient Salvianic acidA loss in the former plant is big, extraction yield is low, the medicinal material waste is big, the time is long, energy consumption is higher, medicine batch differences is big, content is lower.Conventional solvent extraction technology has shortcomings such as big, the consuming time length of solvent load, energy consumption is high, percentage extraction is low; And in extraction process, add the adverse current spray method; With feed liquid through high-pressure fog; Spray the tiny vaporific drop of poling, making it increases with the surface in contact of solvent is long-pending greatly, and the pharmaceutically active ingredient dissolution rate improves 5-6 doubly in can making.Spray method only applied in the dry materials in the past, did not up to the present see the report with the spray method extraction as yet.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of technology of utilizing the spraying counter-current extraction to prepare Salvianic acidA, it is low to have solved the extraction yield that exists in the prior art; The medicinal material waste is big, and the time is long, and energy consumption is higher; The defective that medicine batch differences is bigger, continuous countercurrent adds spraying, has effectively utilized the concentration gradient between two phases; Concentration difference and diffusion area have been increased; Adopt the dynamic circulation mode to carry out, also solved in the traditional extraction technology through adverse current, feed liquid emulsification is not easy stratified drawback.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of technology of utilizing the spraying counter-current extraction to prepare Salvianic acidA may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 20-40 eye mesh screen kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three times extracting solutions merge filtration, and filtrate decompression is concentrated into the fluid extract that proportion is 1.15-1.20;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add diluted mineral acid or organic acid for adjusting pH value, make its pH value, leave standstill then and make the abundant sedimentation of precipitate, remove the solid impurity that occurs after the acidifying with centrifuging for 2.0-5.0;
Wherein used acid can be hydrochloric acid, sulfuric acid, phosphoric acid, formic acid or acetate, and the best is hydrochloric acid or sulfuric acid.
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The mass ratio of feed liquid and ETHYLE ACETATE is 1: effect of extracting was best when 3-5, the pressure of high-pressure fog machine were 2.0-5.0 MPa, flow velocity 200L/h-300L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid adopts vacuum-drying, spraying drying or microwave drying to obtain the Salvianic acidA finished product through being evaporated to the medicinal extract that proportion is 1.15-1.30.
The purpose of acid adjustment: through regulating the pH value in the feed liquid, change the existence of Salvianic acidA, thereby change their partition ratios in solvent, increase extraction efficiency.
Extraction efficiency of the present invention is high, helps making full use of of natural resources of Chinese medicinal materials, and dregs of a decoction utilization ratio is up to 95%, and extraction is complete, and solvent load is little, with short production cycle, the equipment input is little, running cost is low.
The present invention compared with prior art has the following advantages: 1. make Salvianic acidA contained in the red sage root starting material obtain extraction and application to greatest extent; The low medicinal material waste of traditional extraction process extraction yield is big; And use this Technology can make dregs of a decoction utilization ratio up to more than 95%, further reduce production cost, improved the income of enterprise greatly.2. ethyl acetate solvent consumption and solvent consumption reduce significantly, former solvent load be feed liquid 10-12 doubly, the 3-5 that existing consumption is a feed liquid doubly, solvent consumption also reduces greatly, conventional than before extraction solvent consumption reduces more than 60%.3. increase substantially production efficiency; Only need that original production unit is carried out very little renovation and utilization and just can significantly shorten the production cycle; 1 ton of medicinal extract of extraction needs the 4-5d time in the past, and existing with the extraction equipment of the transforming counter-current extraction of spraying, 1 ton of medicinal extract needs the time to be merely 8-12h.4. the recovery of product is elevated to 95% by original 60%, and can make the higher Salvianic acidA of purity, and content can reach more than 50%.5. reduce " waste vapour, waste water, the waste residue " quantity discharged in the production process significantly, the demand of resources such as the organic solvent in the production, water vapor reduces significantly, cuts down the consumption of energy, and reduces air, water resource pollution, has safeguarded good ecotope.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explain.
Embodiment one:
Present embodiment may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 20 eye mesh screens kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three extracting solutions merge and filter, and it is 1.15 fluid extract that filtrate decompression is concentrated into proportion;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add Hydrogen chloride and regulate the pH value, making its pH value is 2.0, leaves standstill 4h then and makes the abundant sedimentation of precipitate, removes the solid impurity that occurs after the acidifying with centrifuging;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 3, and effect of extracting was best when the pressure of high-pressure fog machine was 2.5 MPas, flow velocity 200L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid is 1.2 medicinal extract through being evaporated to proportion, adopts spraying drying to obtain the Salvianic acidA finished product.
The present embodiment assay
The content of Salvianic acidA is 51.2% in the high effective liquid chromatography for measuring sample
Embodiment two
Present embodiment may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 40 eye mesh screens kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three extracting solutions merge and filter, and it is 1.20 fluid extract that filtrate decompression is concentrated into proportion;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add dilute sulphuric acid and regulate the pH value, making its pH value is 3.5, leaves standstill 4h then and makes the abundant sedimentation of precipitate, removes the solid impurity that occurs after the acidifying with centrifuging;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 4, and effect of extracting was best when the pressure of high-pressure fog machine was 4.0 MPas, flow velocity 300L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid is 1.25 medicinal extract through being evaporated to proportion, adopts vacuum-drying to obtain the Salvianic acidA finished product.
The present embodiment assay
The content of Salvianic acidA is 51.8% in the high effective liquid chromatography for measuring sample.
Embodiment three
Present embodiment may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 40 eye mesh screens kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three extracting solutions merge and filter, and it is 1.20 fluid extract that filtrate decompression is concentrated into proportion;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add dilute sulphuric acid and regulate the pH value, making its pH value is 4.5, leaves standstill 4h then and makes the abundant sedimentation of precipitate, removes the solid impurity that occurs after the acidifying with centrifuging;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 5, and effect of extracting was best when the pressure of high-pressure fog machine was 5.0 MPas, flow velocity 300L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid is 1.3 medicinal extract through being evaporated to proportion, adopts microwave drying to obtain the Salvianic acidA finished product.
The present embodiment assay
The content of Salvianic acidA is 52.5% in the high effective liquid chromatography for measuring sample.
The above; Only be three preferable case study on implementation of the present invention; Be not any restriction that the present invention is made, every any simple modification, change, imitation of above case study on implementation being done to technology contents of the present invention all belongs to the protection domain of technical scheme of the present invention.
Claims (5)
1. a technology of utilizing the spraying counter-current extraction to prepare Salvianic acidA is characterized in that, may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 20-40 eye mesh screen kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three times extracting solutions merge filtration, and filtrate decompression is concentrated into the fluid extract that proportion is 1.15-1.20;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add diluted mineral acid or organic acid for adjusting pH value, make its pH value, leave standstill then and make the abundant sedimentation of precipitate, remove the solid impurity that occurs after the acidifying with centrifuging for 2.0-5.0;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 3-5, the pressure of high-pressure fog machine are that 2.0-5.0 MPa, flow velocity are 200L/h-300L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid adopts vacuum-drying, spraying drying or microwave drying to obtain the Salvianic acidA finished product through being evaporated to the medicinal extract that proportion is 1.15-1.30.
2. technology according to claim 1 is characterized in that, described diluted mineral acid of step 3 or organic acid are hydrochloric acid, sulfuric acid, phosphoric acid, formic acid or acetate.
3. technology according to claim 1 is characterized in that, may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 20 eye mesh screens kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three extracting solutions merge and filter, and it is 1.15 fluid extract that filtrate decompression is concentrated into proportion;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add Hydrogen chloride and regulate the pH value, making its pH value is 2.0, leaves standstill 4h then and makes the abundant sedimentation of precipitate, removes the solid impurity that occurs after the acidifying with centrifuging;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 3, and the pressure of high-pressure fog machine is that 2.5 MPas, flow velocity are 200L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid is 1.2 medicinal extract through being evaporated to proportion, adopts spraying drying to obtain the Salvianic acidA finished product.
4. technology according to claim 1 is characterized in that, may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 40 eye mesh screens kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three extracting solutions merge and filter, and it is 1.20 fluid extract that filtrate decompression is concentrated into proportion;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add dilute sulphuric acid and regulate the pH value, making its pH value is 3.5, leaves standstill 4h then and makes the abundant sedimentation of precipitate, removes the solid impurity that occurs after the acidifying with centrifuging;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 4, and the pressure of high-pressure fog machine is that 4.0 MPas, flow velocity are 300L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid is 1.25 medicinal extract through being evaporated to proportion, adopts vacuum-drying to obtain the Salvianic acidA finished product.
5. technology according to claim 1 is characterized in that, may further comprise the steps:
Step 1: medicinal material pre-treatment
Red rooted salvia cleans impurity such as removing silt, oven drying at low temperature or dry after put into built-in 40 eye mesh screens kibbler pulverize;
Step 2: water extraction
The medicinal material that crushes is put in the stainless steel extractor with water boiling and extraction three times; Each 1.5h presses the water that medicinal material weight adds 8 times of amounts for the first time, for the second time with the water that respectively adds 6 times of amounts for the third time; No. three extracting solutions merge and filter, and it is 1.20 fluid extract that filtrate decompression is concentrated into proportion;
Step 3: acidifying feed liquid and solid-liquid separation
In concentrating good fluid extract, add dilute sulphuric acid and regulate the pH value, making its pH value is 4.5, leaves standstill 4h then and makes the abundant sedimentation of precipitate, removes the solid impurity that occurs after the acidifying with centrifuging;
Step 4: spraying counter-current extraction
Step 3 gained feed liquid is dispersed into vaporific droplet under the effect of high-pressure fog machine spray in the extractor; ETHYLE ACETATE then flows into the extractor from the bottom under high-pressure simultaneously; The two fully contacts more complete that extraction is carried out; The ratio of feed liquid and ETHYLE ACETATE is 1: 5, and the pressure of high-pressure fog machine is that 5.0 MPas, flow velocity are 300L/h;
Step 5: extraction liquid concentrate and dry
Extraction liquid is 1.3 medicinal extract through being evaporated to proportion, adopts microwave drying to obtain the Salvianic acidA finished product.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105536290A (en) * | 2015-12-19 | 2016-05-04 | 西安鸿生生物技术有限公司 | Dynamic and continuous atomizing extraction method |
CN110075567A (en) * | 2019-05-28 | 2019-08-02 | 陕西科技大学 | A kind of high-pressure fog combines the centrifugal device and method of adverse current precipitating |
CN113462480A (en) * | 2021-08-16 | 2021-10-01 | 西安鸿生新成生物科技有限公司 | Atomizing distillation process for volatile components in plants |
CN115612185A (en) * | 2022-10-09 | 2023-01-17 | 集美大学 | Preparation method of macroporous rigid agarose gel microspheres |
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CN101289386A (en) * | 2008-06-12 | 2008-10-22 | 南京泽朗医药科技有限公司 | Method for preparing sodium tanshinol |
CN101348474A (en) * | 2007-07-20 | 2009-01-21 | 西安鸿生生物技术有限公司 | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem |
CN101554539A (en) * | 2008-11-21 | 2009-10-14 | 延边大学 | Ultrasonic assistant liquid-liquid spray extraction method |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1586492A (en) * | 2004-07-28 | 2005-03-02 | 张正生 | Medicinal composition containing danshensu, total ara-saponin and camphol and its preparation and use |
CN101348474A (en) * | 2007-07-20 | 2009-01-21 | 西安鸿生生物技术有限公司 | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem |
CN101289386A (en) * | 2008-06-12 | 2008-10-22 | 南京泽朗医药科技有限公司 | Method for preparing sodium tanshinol |
CN101554539A (en) * | 2008-11-21 | 2009-10-14 | 延边大学 | Ultrasonic assistant liquid-liquid spray extraction method |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105536290A (en) * | 2015-12-19 | 2016-05-04 | 西安鸿生生物技术有限公司 | Dynamic and continuous atomizing extraction method |
CN110075567A (en) * | 2019-05-28 | 2019-08-02 | 陕西科技大学 | A kind of high-pressure fog combines the centrifugal device and method of adverse current precipitating |
CN110075567B (en) * | 2019-05-28 | 2021-09-28 | 河北万邦复临药业有限公司 | Centrifugal device and method combining high-pressure spraying with countercurrent sedimentation |
CN113462480A (en) * | 2021-08-16 | 2021-10-01 | 西安鸿生新成生物科技有限公司 | Atomizing distillation process for volatile components in plants |
CN113462480B (en) * | 2021-08-16 | 2024-03-08 | 西安鸿生新成生物科技有限公司 | Atomizing distillation process for volatile components in plants |
CN115612185A (en) * | 2022-10-09 | 2023-01-17 | 集美大学 | Preparation method of macroporous rigid agarose gel microspheres |
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Application publication date: 20120926 |