CN101530449B - Method of preparing honeysuckle extract by applying membrane filtration technology - Google Patents
Method of preparing honeysuckle extract by applying membrane filtration technology Download PDFInfo
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- CN101530449B CN101530449B CN2008100430517A CN200810043051A CN101530449B CN 101530449 B CN101530449 B CN 101530449B CN 2008100430517 A CN2008100430517 A CN 2008100430517A CN 200810043051 A CN200810043051 A CN 200810043051A CN 101530449 B CN101530449 B CN 101530449B
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Abstract
The invention provides a method of preparing a honeysuckle extract by applying membrane filtration technology, comprising the steps of: firstly extracting the honeysuckle by adding water and decoction; implementing decompression, concentration and centrifugation; removing most of impurities with a micro-filtration membrane; and further implementing refining with an ultra-filtration membrane. Compared with the prior art, the method not only can guarantee the extraction of the effective components of honeysuckle, but also can reduce the leaching of impurities, can effectively remove the impurities, reduce the sensitized components and improve the total content of the effective components. Therefore, the method can overcome the shortcomings of the prior art, has simple operation and high recovery rate of separated materials, and can also provide process conditions which are more conducive to the industrial production.
Description
Technical field
The present invention relates to a kind of Chinese medicinal preparation method, relate in particular to a kind of method for extraction and purification of middle pharmaceutically active ingredient, be specifically related to a kind of method of preparing honeysuckle extract by applying membrane filtration technology.
Background technology
Flos Lonicerae is the dry flower of caprifoliaceae plant Radix Ophiopogonis Lonicera japonica Thunb., Flos Lonicerae Lonicera hypoglauca Miq., Flos Lonicerae Lonicera confuse DC. or hair style Radix Ophiopogonis Lonicera dasytyla Rehd. or the flower that band is just opened.Flos Lonicerae is conventional Chinese medicine, and is cold in nature, and sweet in the mouth has remarkable heat-clearing and toxic substances removing, anti-inflammation and antivirus action, and wind-heat dissipating is used for carbuncle furuncle, sore throat, erysipelas, warm blood fulminant dysentery, anemopyretic cold, epidemic febrile disease heating.
Flos Lonicerae is contained to be that the organic acid composition of representative is its main effective ingredient with the chlorogenic acid.The method of from Flos Lonicerae, extracting the organic acid composition at present adopts warm macerating method, water-boiling method, rare alcohol extraction and acid alcohol extraction etc. usually, and purification process adopts alcohol deposition method, water alcohol method, stone mercaptans, extraction, macroreticular resin absorbing method etc. more; Wherein alcohol deposition method and water precipitating method can only reach the purpose of preliminary purification, and it is big that it receives the cream amount, and organic acid content is low.Stone sulfur method, extraction and macroreticular resin absorbing method are used separately respectively the higher preparation of ask for something are yet existed some shortcomings, such as, stone sulfur method possibly brought some metal ions into; The extraction pigment is more, and extract viscosity is big, makes the preparation color darker; Macroreticular resin absorbing method needs repeated treatments, troublesome poeration, and repeatability is relatively poor; And having organic residue problem, these have directly influenced the safety and the stability of preparation.
In state-owned many pieces of patents introduce the Flos Lonicerae extract method for preparing, but all exist to receive higher, the problems such as content is lower, the rate of transform is low, complicated operation of cream rate.
Summary of the invention
The technical problem that the present invention will solve provides a kind of method of preparing honeysuckle extract by applying membrane filtration technology; Be used for solving technical problems such as the present Flos Lonicerae extraction process chlorogenic acid rate of transform is low, technology cost height, preparation process poor stability, the present invention realizes through following technical scheme:
The present invention provides a kind of method for preparing of Flos Lonicerae extract, and this method may further comprise the steps:
(1) decoct extraction: the extracting honeysuckle medical material, add water and decocted 1-2 hour, leaching medicinal liquid, medicinal residues decocte with water 0.5-1 hour again, the leaching medicinal liquid discards medicinal residues; Merge medicinal liquid twice, medicinal liquid is concentrated into relative density 1.0-1.1 (60 ℃ of surveys), be cooled to room temperature and get decoction liquor;
(2) crude separation: with the decoction liquor centrifugalize, rotating speed 4000-6000 rev/min, centrifugal 10-20 minute, get supernatant, carry out micro-filtration membrane and separate, the control flow velocity is 5～10ml/min, and carries out filter wash with distilled water or purified water, merging filtrate gets crude extract;
(3) refining: crude extract is carried out ultrafilter membrane separate, control flow velocity 1～5ml/min, and carry out filter wash with distilled water or purified water, merging filtrate, concentrating under reduced pressure, vacuum drying promptly gets Flos Lonicerae extract.
Hydromining is with purified water, distilled water or water for injection described in the step (1).Step (1) in the inventive method decocts in the extraction, generally all is to adopt purified water, distilled water or water for injection to decoct, and this mainly is in order to meet the needs of clinical drug safety.The 8wt-18wt times of water gaging that its amount of water that decocts for the first time is a decocting herbs weight, the amount of water that decocts for the second time is a 6wt-12wt times of water gaging of decocting herbs weight.Extract temperature and generally be controlled at 95 ℃, keep little the boiling of solution to get final product.
Employed micro-filtration membrane micro-filtration membrane specification is 0.42-0.65micron or 50000-300000NMWC in the step (2), and flow velocity is 5～10ml/min, and carries out 2-5 time distilled water or purified water filter wash, and effective ingredient such as assurance chlorogenic acid see through rete as far as possible.
Employed ultrafilter membrane specification is 1000-30000NMWC in the step (3), and flow velocity is 1～5ml/min, and carries out 2-5 time distilled water or purified water filter wash, and effective ingredient such as assurance chlorogenic acid see through rete as far as possible.Adopt concentrating under reduced pressure when concentrating, the dry vacuum drying that adopts, temperature all is controlled at 50-70 ℃, to guarantee the decomposes of effective ingredient such as chlorogenic acid.
Membrance separation (membrane filtration) technology is an emerging high efficient separation technology, by internationally recognized be a most rising great high production tech of mid-term 20 end of the centurys to 21 century.Hyperfiltration technique is a kind of membrane separation technique that grows up 60～seventies of 20th century, and it is to use the porous semipermeable membrane to be medium, filters with the cross-flow mode.The aperture of ultrafilter membrane is minimum, can stop various microgranules, colloid and macromole solute in the solution, to reach the purpose of concentrated or purification and impurity removal.Compare advantage such as ultrafiltration has the conversion that needn't pass through phase, need not add chemical reagent, filter membrane is difficult for stopping up and durable with common separation method.
According to chemical property and structure, membrane material can be divided into two big types: organic membrane and inoranic membrane.Facts have proved that organic membrane exists all the time can not solve film and pollute, can not resist problems such as high pressure and high temperature; So people begin to make many shortcomings that inorganic separating film and material thereof remedy organic membrane, so the inoranic membrane separation equipment has a extensive future in Chinese medicine extraction is separated.
Compared with prior art, the present invention has following beneficial effect: based on technique scheme, the applicant confirms through overtesting; If adopt membrane filtration technique to prepare Flos Lonicerae extract, can significantly improve content of effective in the Flos Lonicerae extract, improve the rate of transform of chlorogenic acid; Not only can practice thrift the medical material cost; More can simplify the commercial production step, simple to operate, the process conditions that more help commercial production ground can be provided; And guarantee the stability and the safety of technology to make this Chinese medicine bring into play its effect as far as possible.Characteristics of the present invention are: when Flos Lonicerae was extracted, little boiling got final product, and can guarantee the extraction of effective ingredient like this, can reduce the stripping of impurity again; Can remove impurity effectively, reduce the sensitization composition, and total content of effective is improved.The method that adopts microfiltration and ultrafiltration to combine can effectively be removed invalid components such as resin, tannin, phlegmatic temperament, pigment, avoids the use of organic reagent simultaneously and reduces the commercial production pollution; The more important thing is that having avoided chlorogenic acid is the main loss of organic acid active component in other complicated preparation technology, this method can make the chlorogenic acid rate of transform reach more than 90%, can maximize the medical value that improves Chinese medicine honeysuckle.
The specific embodiment
Below further specify the present invention through embodiment, but should be understood that these embodiment are exemplary, the present invention is not limited thereto.
Embodiment 1:
Take by weighing Flos Lonicerae 200g, add 12 times of little decoctions of boiling of water 2400ml (95 ℃) 1.5 hours, filter, medicinal residues add 10 times of little decoctions of boiling of water 2000ml (95 ℃) 1.0 hours, filter, and merging filtrate is divided into two parts, and portion carries out membrane filtration to be separated, and portion carries out precipitate with ethanol to be separated.
1. membrane filtration separates: get extracting solution, 60 ℃ are evaporated to proportion is 1.05 (60 ℃), and centrifugal 15 minutes of 4500 rev/mins speed is got supernatant, crosses micro-filtration membrane (0.65Micron), control flow velocity 10ml/min, and with distilled water filter wash 3 times, 100ml at every turn; Micro-filtrate is crossed ultrafilter membrane (10000NMWC), and the control flow velocity is 5ml/min, with distilled water filter wash 3 times, and each 50ml, it is 1.2 (60 ℃) that 60 ℃ of ultrafiltrates are evaporated to proportion, vacuum drying obtains Flos Lonicerae extract dry powder.
2. precipitate with ethanol separates: get extracting solution, 60 ℃ are evaporated to proportion is 1.15 (60 ℃), and adding 95% ethanol is 80% to containing the alcohol amount, stir, and hold over night, the centrifugal supernatant that obtains reclaims ethanol, and vacuum drying gets the Flos Lonicerae extract that alcohol precipitation process makes.
3. testing result
3.1 the chlorogenic acid content and the rate of transform:
The sample title chlorogenic acid content dry extract yield chlorogenic acid rate of transform
Membrane filtration process 70% 4% 92%
Alcohol precipitation process 12% 8% 36%
3.2 membrane filtration cost analysis table
Technology category time consumptive material technical process
Membrane filtration process rate of filtration 5ml/min film material filters, concentrates
Alcohol precipitation process need leave standstill generally that 12-24hr 95% ethanol concentrates, precipitate with ethanol, concentrate
For Flos Lonicerae, serve as to investigate index with main functional component chlorogenic acid, the membrane filtration process rate of transform is high, and technical process is simple, can remove macromolecular starch, saccharide, tannin, chlorophyll etc. basically.In addition, the membrane filtration production cost is low than alcohol precipitation process, and production environment is more excellent, and can shorten the production cycle, helps applying of this technology.Above contrast experiment will adopt membrane filtration process of the present invention to prepare Flos Lonicerae extract with employing traditional handicraft alcohol precipitation process and compare, and experimental result has demonstrated fully high efficiency, low cost, low pollution, the high rate of transform, the highly purified advantage that adopts membrane filtration process of the present invention to prepare Flos Lonicerae extract.
Embodiment 2:
Take by weighing Flos Lonicerae 200g, add 8 times of little decoctions of boiling of water 1600ml (95 ℃) 1 hour, filter, medicinal residues add 6 times of little decoctions of boiling of water 1200ml (95 ℃) 0.5 hour; Filter, merging filtrate, will filtrate 60 ℃ and be evaporated to proportion is 1.05 (60 ℃); Centrifugal 20 minutes of 4000 rev/mins speed is got supernatant, crosses micro-filtration membrane (0.42Micron); Control flow velocity 5ml/min, with distilled water filter wash 2 times, 100ml at every turn; Micro-filtrate is crossed ultrafilter membrane (1000NMWC), and the control flow velocity is 1ml/min, with distilled water filter wash 2 times, and each 50ml, it is 1.2 (60 ℃) that 60 ℃ of ultrafiltrates are evaporated to proportion, vacuum drying obtains Flos Lonicerae extract dry powder.
Embodiment 3:
Take by weighing Flos Lonicerae 200g, add 18 times of little decoctions of boiling of water 3600ml (95 ℃) 2 hours, filter, medicinal residues add 12 times of little decoctions of boiling of water 2400ml (95 ℃) 0.8 hour; Filter, merging filtrate, will filtrate 60 ℃ and be evaporated to proportion is 1.0 (60 ℃); Centrifugal 15 minutes of 5000 rev/mins speed is got supernatant, crosses micro-filtration membrane (0.5Micron); Control flow velocity 7ml/min, with distilled water filter wash 5 times, 100ml at every turn; Micro-filtrate is crossed ultrafilter membrane (30000NMWC), and the control flow velocity is 3ml/min, with distilled water filter wash 5 times, and each 50ml, it is 1.2 (60 ℃) that 60 ℃ of ultrafiltrates are evaporated to proportion, vacuum drying obtains Flos Lonicerae extract dry powder.
Embodiment 4:
Take by weighing Flos Lonicerae 200g, add 15 times of little decoctions of boiling of water 3000ml (95 ℃) 1.5 hours, filter, medicinal residues add 10 times of little decoctions of boiling of water 2000ml (95 ℃) 0.8 hour; Filter, merging filtrate, will filtrate 60 ℃ and be evaporated to proportion is 1.1 (60 ℃); Centrifugal 10 minutes of 6000 rev/mins speed is got supernatant, crosses micro-filtration membrane (0.5Micron); Control flow velocity 8ml/min, with distilled water filter wash 3 times, 100ml at every turn; Micro-filtrate is crossed ultrafilter membrane (20000NMWC), and the control flow velocity is 3ml/min, with distilled water filter wash 3 times, and each 50ml, it is 1.2 (60 ℃) that 60 ℃ of ultrafiltrates are evaporated to proportion, vacuum drying obtains Flos Lonicerae extract dry powder.
Claims (4)
1. the method for a preparing honeysuckle extract by applying membrane filtration technology, this method may further comprise the steps:
(1) decoct extraction: the extracting honeysuckle medical material, add water and decocted 1-2 hour, leaching medicinal liquid, medicinal residues decocte with water 0.5-1 hour again, the leaching medicinal liquid discards medicinal residues; Merge medicinal liquid twice, medicinal liquid is concentrated into relative density 1.0-1.1, be cooled to room temperature and get decoction liquor;
(2) crude separation: with the decoction liquor centrifugalize, rotating speed 4000-6000 rev/min, centrifugal 10-20 minute; Get supernatant, carry out micro-filtration membrane and separate, employed micro-filtration membrane specification is 0.42-0.65micron or 50000-300000NMWC; The control flow velocity is 5～10ml/min; And carry out filter wash with distilled water or purified water, merging filtrate, crude extract;
(3) refining: crude extract is carried out ultrafilter membrane separate, employed ultrafilter membrane specification is 1000-30000NMWC, controls flow velocity 1～5ml/min, and carries out filter wash with distilled water or purified water, merging filtrate, and concentrating under reduced pressure, vacuum drying promptly gets Flos Lonicerae extract.
2. the method for preparing honeysuckle extract by applying membrane filtration technology according to claim 1 is characterized in that, hydromining is with purified water, distilled water or water for injection described in the step (1).
3. the method for preparing honeysuckle extract by applying membrane filtration technology according to claim 1 and 2; It is characterized in that; In step (1); The amount of water that decocts for the first time is a 8wt-18wt times of water gaging of decocting herbs weight, and the amount of water that decocts for the second time is a 6wt-12wt times of water gaging of decocting herbs weight.
4. the method for preparing honeysuckle extract by applying membrane filtration technology according to claim 1 is characterized in that, in step (2), the filter wash number of times was 2-5 time during micro-filtration membrane was separated; In step (3), the filter wash number of times was 2-5 time during ultrafilter membrane separated.
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| CN102145037A (en) * | 2010-02-04 | 2011-08-10 | 天津天士力现代中药资源有限公司 | Method for drying honeysuckle extract |
| CN103102270A (en) * | 2011-11-09 | 2013-05-15 | 安康市天源植物提取有限公司 | Preparation method of chlorogenic acid |
| CN104845405A (en) * | 2014-02-17 | 2015-08-19 | 山东禾本堂生物科技有限公司 | Process for extracting honeysuckle dye from honeysuckle |
| CN108030798A (en) * | 2017-12-12 | 2018-05-15 | 广东广发制药有限公司 | Honeysuckle extracting method, honeysuckle dried cream powder and honeysuckle detoxicating capsule and preparation method |
| CN110903191A (en) * | 2018-09-17 | 2020-03-24 | 泰州医药城国科化物生物医药科技有限公司 | Method for extracting chlorogenic acid from honeysuckle |
| CN110898095A (en) * | 2018-09-17 | 2020-03-24 | 泰州医药城国科化物生物医药科技有限公司 | Honeysuckle refined product and preparation method and application thereof |
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| 刘振丽等.超滤及醇沉对金银花中绿原酸的影响.《中成药》.1996,第18卷(第2期),4-6. * |
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