CN102001946B - Novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower - Google Patents
Novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower Download PDFInfo
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- CN102001946B CN102001946B CN201010540206.5A CN201010540206A CN102001946B CN 102001946 B CN102001946 B CN 102001946B CN 201010540206 A CN201010540206 A CN 201010540206A CN 102001946 B CN102001946 B CN 102001946B
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Abstract
The invention relates to a novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower by wall-breaking ultrasonic extraction separation technology. The method comprises the following steps of: performing wall-breaking treatment by adopting a high-frequency vibration wall-breaking crusher, and performing ultrasonic water extraction filtration; standing and refrigerating filtrate, and centrifugally filtering to obtain an oil-water mixture; centrifuging the oil-water mixture at a high speed again; performing ultrafiltration on a water phase, extracting by using ethyl acetate, and separating, concentrating and drying to obtain high-purity chlorogenic acid; and performing molecular distillation on an oil phase to prepare high-quality honeysuckle flower essential oil. The method furthest ensures the bioactivity and original characteristics of active ingredients, greatly improves the utilization rate of a honeysuckle flower resource and can remarkably save energy and reduce pollution. The honeysuckle flower treated by unique methods such as wall-breaking ultrasonic extraction and the like can be used to simultaneously prepare high-purity and high-quality chlorogenic acid and honeysuckle flower essential oil, which are widely applied to food, medicines, cosmetics and commodities, so that the aim of fully utilizing resources is fulfilled and the method has good economic benefits.
Description
Technical field
The present invention relates to the extraction process of bioactive ingredients, refer in particular to a kind of broken wall supersound extraction isolation technique of utilizing and extract and the novel method that separates Chlorogenic Acid of Flos Lonicerae and Japanese Honeysuckle essential oil simultaneously.
Background technology
Japanese Honeysuckle, gas is fragrant strongly fragrant and taste is sweet.Its extract chlorogenic acid is a kind of important biologically active substance, have antibacterial, antiviral, increase the effects such as white cell, hepatic cholagogic, antitumor, hypotensive, reducing blood-fat, removing free radical and stimulating central nervous system system.The Rose Absolute of Japanese Honeysuckle is applied very extensive in food, medicine, makeup, daily necessities.
The extraction prior art of Chlorogenic Acid of Flos Lonicerae adopts ethanol repeatedly to extract the rear and then various impurity removing technology purification chlorogenic acids of process more: extraction time is long, effective constituent is easily destroyed; Need to use organic solvent, cost is higher; In impurity elimination purge process because precipitation capacity causes greatly filtration difficulty, chlorogenic acid yield and purity not high; Be difficult for realizing commercial production scale.After the preparation of Japanese Honeysuckle essential oil adopts wet distillation more, organic solvent extracts again, and essential oil yield is low.In Japanese Honeysuckle, contain the material of many thermo-sensitivitys, can be destroyed under the effect of pyrogenic distillation or decoction, and also most nonvolatile functional mass stays in mother liquor and is dropped, and causes Japanese Honeysuckle proper constituent disappearance, and medicinal ingredients destroys more serious.And tradition extract the process in leaching of bioactive ingredients be one by cell walls, cytolemma dissolve, the process of infiltration, diffusion, thereby traditional extraction technique needs High Temperature High Pressure, a large amount of solvent, repeatedly extracts.Extracts active ingredients insufficient and easily destroyed, consume a large amount of raw materials and energy, contaminate environment.The existing extractive technique of Japanese Honeysuckle or only utilized chlorogenic acid or Japanese Honeysuckle essential oil wherein, other compositions are dropped, and its preparation method lacks due comprehensive utilization.China's natural resources of Chinese medicinal materials present situation allows of no optimist, and Chinese medicinal materials supply is becoming tight day, but also has this painful serious wasting of resources phenomenon in Japanese Honeysuckle produces: according to estimates, the Japanese Honeysuckle of causing for a year wastes up to 20,000 tons.
Summary of the invention
The object of the invention is for the shortcoming existing in background technology and problem improvement and bring new ideas in addition, a kind of utilization ratio that can improve to the utmost effective constituent in Japanese Honeysuckle is provided, prevent that an a kind of or effective constituents and discarded other compositions that enterprise only extracts in Japanese Honeysuckle from causing the wasting of resources, solve that production technique energy consumption is in the past large simultaneously, extract and the novel method that separates Chlorogenic Acid of Flos Lonicerae and Japanese Honeysuckle essential oil when problem of environmental pollution.
The inventive method adopts broken wall supersound extraction isolation technique to prepare two products of Japanese Honeysuckle simultaneously, i.e. chlorogenic acid and Japanese Honeysuckle essential oil, and described broken wall supersound extraction isolation technique specifically comprises the following steps:
1) start of high-frequency vibration wall-broken grinder is chilled to-20～-60 ℃ in advance;
2) with high frequency wall-broken grinder, Japanese Honeysuckle wall cell disruption powder is broken to 5-50 micron, Japanese Honeysuckle cell wall breaking rate reaches 50%～90%;
3) add 2～5 times of water gagings, under 10～60KHz ul-trasonic irradiation, normal temperature lixiviate 20～60 minutes;
4) refrigeration leaves standstill 10～48 hours, if the existing oil reservoir in surface can first take out, obtains the thick essential oil of part, then elimination precipitation, obtains oil-water mixture;
5) utilize supercentrifuge separating oil water mixed liquid, obtain the thick oil of Japanese Honeysuckle and water extract of flos lonicerae;
6) thick Japanese Honeysuckle oil is carried out to molecular distillation at 60～100 ℃, obtain high-quality Japanese Honeysuckle essential oil;
7) water extract of flos lonicerae, adding HCl tune PH is 2.0～4.0, ultrafiltration, with ethyl acetate extraction, acetic acid ethyl fluid activated carbon decolorizing, filters, and after filtrate is concentrated, drying under reduced pressure, obtains chlorogenic acid fine work, and content reaches more than 95%.
Supercentrifuge of the present invention is the above supercentrifuge of 3000r/min.
Ultrafiltration of the present invention is the following ultrafiltration of 10000 molecular weight.
Advantage of the present invention and beneficial effect:
1, technique is more scientific, reasonable.After the extraction prior art of Chlorogenic Acid of Flos Lonicerae adopts ethanol repeatedly to extract more and then through various impurity removing technology purification chlorogenic acids; After the preparation of Japanese Honeysuckle essential oil adopts wet distillation more, organic solvent extracts again, and essential oil yield is low.In Japanese Honeysuckle, contain the material of many thermo-sensitivitys, can be destroyed under the effect of pyrogenic distillation or decoction, and also most nonvolatile functional mass stays in mother liquor and is dropped, and causes Japanese Honeysuckle proper constituent disappearance, and medicinal ingredients destroys more serious.Japanese Honeysuckle adopts broken wall and ultrasonic lixiviate, extraction conditions gentleness, and purifying process is more reasonable, when greatly limit is extracted wherein effective constituent, has effectively protected wherein bioactive ingredients.
2, the utilization of resources is abundant.Japanese Honeysuckle is as a kind of Chinese medicine, and its composition is very complicated, mainly take chlorogenic acid, phyllyrin, Flavonoid substances as representative." Chinese Pharmacopoeia " sign material using the chlorogenic acid in Japanese Honeysuckle as Japanese Honeysuckle is main effect material of Japanese Honeysuckle; The fragrance of a flower smell of Japanese Honeysuckle is mainly derived from its lower boiling volatile constituent, can obtain highly purified fragrant Japanese Honeysuckle essential oil by molecular distillation.The present invention has utilized resource to greatest extent, has great importance from Chinese medicine conservation of resources angle.
3, less energy-consumption, environmental protection and energy saving.Traditional extraction technique needs High Temperature High Pressure, a large amount of solvent, repeatedly extracts, and production technique energy consumption is large, contaminate environment.And this technique only adopts the ultrasonic water extraction of low temperature high-frequency vibration pulverize and break cellular wall technology, solvent is few, extraction rate is fast, power consumption is few, without hazardous solvent, save energy, protected environment.
4, quality-advantage.Chlorogenic acid and two kinds of products of essential oil that Japanese Honeysuckle adopts advanced broken wall supersound extraction to obtain, improved the utilization ratio of effective constituent in Japanese Honeysuckle to the utmost, utilizes advanced HPLC method to detect its effective constituent, and the yield of chlorogenic acid reaches more than 95%; Essential oil is light yellow liquid, and main chemical compositions has all reached documentation standards as phantol, terpinol, linalool monoxide, the various indexs of Geraniol.Thereby quality and the curative effect of product are guaranteed.
Broken wall supersound extraction isolation technique of the present invention be one based on modern plants broken wall, the modern biotechnologies such as ultrasonic lixiviate and active ingredient of natural product researching and developing extract and separate new technique, its novelty is: substitute high temperature with the ultrasonic extracting technology of normal temperature after plant cell wall breaking and decoct, concentrated, evaporation, the traditional technologys such as backflow, greatly simplify technological process, biological activity and the ecosystem feature of effective constituent are farthest guaranteed, avoid the destruction of High Temperature High Pressure to effective ingredient of honeysuckle in traditional extraction concentration technique, greatly improve Japanese Honeysuckle resource utilization, and remarkable save energy, reduce and pollute.Adopt the peculiar methods such as broken wall supersound extraction to process can to prepare after Japanese Honeysuckle in food, medicine, makeup, daily necessities application chlorogenic acid and the Japanese Honeysuckle essential oil of high purity and high-quality very widely simultaneously, thereby reach the object that makes full use of resource, and there is good economic benefit.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Specific embodiment:
1) first the start of high-frequency vibration wall-broken grinder is chilled to-40 ℃ in advance;
2) with high frequency wall-broken grinder, Japanese Honeysuckle wall cell disruption powder is broken to 30 microns, Japanese Honeysuckle cell wall breaking rate reaches 90%;
3) add 4 times of water gagings, under 30KHz ul-trasonic irradiation, normal temperature lixiviate 40 minutes;
4) refrigeration leaves standstill 28 hours, and existing surface oil reservoir is taken out, and obtains the thick essential oil of part, then elimination precipitation, obtains oil-water mixture; Separately throw out is dried as fodder additives;
5) utilize 3000r/min supercentrifuge separating oil water mixed liquid, obtain the thick oil of Japanese Honeysuckle and water extract of flos lonicerae;
6) thick Japanese Honeysuckle oil is carried out to molecular distillation at 80 ℃, obtain high-quality Japanese Honeysuckle essential oil;
7) water extract of flos lonicerae, adding HCl tune PH is 3.0,8000 molecular weight ultrafiltration, and with ethyl acetate extraction, acetic acid ethyl fluid activated carbon decolorizing, filters, and after filtrate is concentrated, drying under reduced pressure, obtains chlorogenic acid fine work, and content reaches 98%.
Technological principle of the present invention:
The invention discloses a kind of method of extracting high-purity chlorogenic acid and fragrant Japanese Honeysuckle essential oil from Japanese Honeysuckle, its technology contents is that after Japanese Honeysuckle is adopted to high-frequency vibration wall-broken grinder broken wall treatment, ultrasonic wave water extraction is filtered, after filtered liquid leaves standstill refrigeration, centrifugal filtering obtains oil-water mixture, oil-water mixture is high speed centrifugation again, to after water ultrafiltration, be extracted with ethyl acetate, separate concentrate drying, obtain high-purity chlorogenic acid, and oil phase is prepared the Japanese Honeysuckle essential oil of high-quality by molecular distillation.The present invention adopts broken wall ultrasonic technique to prepare chlorogenic acid and Japanese Honeysuckle essential oil.
Cell wall breaking extract be phalangeal cell after physical wall breaking, add the technique of the required bioactive ingredients of solvent lixiviate stripping.Because cell is after physical wall breaking, cell walls is broken completely to the obstruction of effective constituent, therefore, in cell wall breaking extraction process the extraction process in leaching of bioactive ingredients actual be exactly the direct process in leaching of solvent to required bioactive ingredients, effective constituent stripping is rapidly and completely.
In recent years, rapidly, from laboratory study to large-scale production, application transforms the development of plant wall breaking technology just gradually.At present, technology maturation and in scale production the plant wall breaking technology of widespread use have two kinds, the one, low temperature supersonic airstream wall breaking technology, the one, low temperature high-frequency vibration wall breaking technology.Research shows that low temperature high-frequency vibration pulverizer is good to Japanese Honeysuckle shell-broken effect by experiment.High-frequency vibration broken wall crushing technology is that the reactive forces such as the impact that utilizes spherical or clavate mill to be situated between to make high-frequency vibration and produce, friction, shearing are realized the broken wall of material is pulverized.Spring supporting grinding machine body for vibration mill, makes its vibration by one with the main shaft of eccentric block, the normally cylindrical or flute profile of grinding machine.The common mill of efficiency ratio of vibration mill is high 10～20 times, and its grinding speed is more faster than conventional ball mill, and the low several times of energy consumption.Cell wall breaking extract actual be the direct process in leaching of a bioactive ingredients after broken wall, thereby, extraction conditions gentleness, solvent is few, extraction rate is fast, resource utilization is high, extract quality of finished product good.This just cell wall breaking extractive technique effective component extraction rate, extraction rate higher than the theoretical basis of traditional extraction technology.
Under the wall breaking technology of Japanese Honeysuckle, adopt ultrasonic wave to extract two kinds of products such as preparing Chlorogenic Acid of Flos Lonicerae simultaneously.In recent years, the application of ultrasonic technology in plant extract technique more and more receives publicity.Ultrasonic extraction is the mechanical effect that utilizes ultrasonic wave to have, cavitation effect and heat effect, by increase medium molecule movement velocity, increase medium penetration power with extract biological effective components.Ultrasonic extraction has following advantage: increase the sporoderm-broken rate of Japanese Honeysuckle, do not need heating; Improve the extraction yield of effective ingredient; Solvent load is few; Do not affect the physiologically active of most drug effective constituent.The present invention adopt broken wall and the method for ultrasonic wave combination extract that products such as separating Chlorogenic Acid of Flos Lonicerae has technique advanced person, scientific and reasonable, easy and simple to handle, cost is low, without hazardous solvent, purity is high, yield is high, the utilization of resources fully, be applicable to the advantages such as industrialized mass.
Embodiment of the present invention is only the description that the preferred embodiment of the present invention is carried out; not design of the present invention and scope are limited; do not departing under the prerequisite of design philosophy of the present invention; various modification and improvement that in this area, engineering technical personnel make technical scheme of the present invention; all should fall into protection scope of the present invention; the technology contents of request protection of the present invention, has all been documented in claims.
Claims (3)
1. one kind is extracted and the method that separates Chlorogenic Acid of Flos Lonicerae and Japanese Honeysuckle essential oil simultaneously, it is characterized in that the method adopts broken wall supersound extraction isolation technique to prepare two products of Japanese Honeysuckle simultaneously, be chlorogenic acid and Japanese Honeysuckle essential oil, described broken wall supersound extraction isolation technique specifically comprises the following steps:
1) start of high-frequency vibration wall-broken grinder is chilled to-20～-60 ℃ in advance;
2) with high frequency wall-broken grinder, Japanese Honeysuckle wall cell disruption powder is broken to 5-50 micron, Japanese Honeysuckle cell wall breaking rate reaches 50%～90%;
3) add 2～5 times of water gagings, under 10～60KHz ul-trasonic irradiation, normal temperature lixiviate 20～60 minutes;
4) refrigeration leaves standstill 10～48 hours, if the existing oil reservoir in surface can first take out, obtains the thick essential oil of part, then elimination precipitation, obtains oil-water mixture;
5) utilize supercentrifuge separating oil water mixed liquid, obtain the thick oil of Japanese Honeysuckle and water extract of flos lonicerae;
6) thick Japanese Honeysuckle oil is carried out to molecular distillation at 60～100 ℃, obtain Japanese Honeysuckle essential oil;
7) water extract of flos lonicerae, adding HCl tune pH is 2.0～4.0, ultrafiltration, with ethyl acetate extraction, acetic acid ethyl fluid activated carbon decolorizing, filters, and after filtrate is concentrated, drying under reduced pressure, obtains chlorogenic acid fine work, and content reaches more than 95%.
2. a kind of simultaneously extraction and the method that separates Chlorogenic Acid of Flos Lonicerae and Japanese Honeysuckle essential oil according to claim 1, is characterized in that described supercentrifuge is the above supercentrifuge of 3000r/min.
3. a kind of simultaneously extraction and the method that separates Chlorogenic Acid of Flos Lonicerae and Japanese Honeysuckle essential oil according to claim 1, is characterized in that described ultrafiltration is the following ultrafiltration of 10000 molecular weight.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN104058966B (en) * | 2014-06-26 | 2016-05-25 | 正安县黔蕊茶业有限公司 | A kind of from honeysuckle the device of chlorogenic acid extracting |
| CN104830531A (en) * | 2015-04-29 | 2015-08-12 | 绥阳县吉帮金银花科技发展有限公司 | Wild honeysuckle flower essential oil and preparation method thereof |
| CN105192876B (en) * | 2015-10-20 | 2021-05-28 | 贵州中烟工业有限责任公司 | Buccal smokeless tobacco composition added with plant composition and application thereof |
| CN106221916B (en) * | 2016-07-22 | 2019-10-25 | 深圳波顿香料有限公司 | A kind of extracting method and its extract, application of Chinese prickly ash fragrance ingredient |
| CN106256344A (en) * | 2016-08-30 | 2016-12-28 | 郭清辉 | A kind of Flos Lonicerae quintessence oil dew and preparation method thereof |
| CN109430645A (en) * | 2018-11-15 | 2019-03-08 | 湖北大别山药业股份有限公司 | A kind of novel honeysuckle compound beverage and preparation method thereof |
| CN109852479B (en) * | 2019-03-05 | 2022-02-01 | 云南中烟新材料科技有限公司 | Method for preparing flue-cured tobacco absolute oil by oil bleaching method and application thereof |
| CN110157544A (en) * | 2019-05-20 | 2019-08-23 | 山东省分析测试中心 | A kind of total preparation facilities and method of the distilled liquid of honeysuckle and water extract of flos lonicerae |
| CN117398322A (en) * | 2023-12-13 | 2024-01-16 | 广州悦瑞化妆品有限公司 | Microbead essence and preparation method thereof |
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Denomination of invention: A method for simultaneous extraction and separation of chlorogenic acid and honeysuckle essential oil from honeysuckle Effective date of registration: 20220701 Granted publication date: 20140625 Pledgee: Agricultural Bank of China Limited Linxiang sub branch Pledgor: HUNAN RHON PHARMACEUTICAL Co.,Ltd. Registration number: Y2022980009698 |