CN102476996A - Extraction process of chlorogenic acid in honeysuckle - Google Patents
Extraction process of chlorogenic acid in honeysuckle Download PDFInfo
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- CN102476996A CN102476996A CN2010105522546A CN201010552254A CN102476996A CN 102476996 A CN102476996 A CN 102476996A CN 2010105522546 A CN2010105522546 A CN 2010105522546A CN 201010552254 A CN201010552254 A CN 201010552254A CN 102476996 A CN102476996 A CN 102476996A
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Abstract
An extraction process of chlorogenic acid in honeysuckle relates to an extraction process of chlorogenic acid and has few extraction steps and high extraction rate. The technical scheme includes that the chlorogenic acid in the honeysuckle is extracted by an alcohol backflow method, and the extraction process includes steps that microwave treatment is carried out, the honeysuckle is filled in a special 250ml microwave container provided with a condenser, and is pre-soaked for 8 to 24 hours, the power of microwaves is set to a range from 600W to 800W, radiation time is 1-3min, a microwave oven is started, and extract is combined after extraction and is concentrated and dried to obtain crude extract; enzymolysis extraction is carried out, 0-3.0% of enzymatic hydrolysate is added into the crude extract, the enzymolysis temperature ranges from 25 DEG C to 60 DEG C, enzymolysis is carried out for 1 to 4 hours, alcohol with added material liquid ratio of 1:8 to 1:12, the concentration of the alcohol ranges from 65% to 75%, and backflow digestion is carried out for 0.5 to 1.5 hours; and the chlorogenic acid is purified.
Description
Technical field:
The present invention relates to a kind of extraction process of chlorogenicacid, more particularly, relate to the extraction process of chlorogenicacid in the Japanese Honeysuckle.
Background technology:
Japanese Honeysuckle is the caprifoliaceae plant dry flower of honeysuckle, is one of clinical Chinese medicinal materials commonly used, has the function of clearing heat and detoxicating, cool breeze heat radiation, antiviral, hepatic cholagogic.Recent study is found, is rich in the multiple material useful to HUMAN HEALTH in the Japanese Honeysuckle, such as volatile oil, flavones and chlorogenic acid, triterpenes and trace element etc., has very high utility value.Chlorogenicacid comparatively enriches and has the various active function in numerous compositions, therefore often estimates the quality of Japanese Honeysuckle quality with the height of chlorogenic acid content.Chlorogenicacid also has flavouring and color-protecting function, can be used for food and fruit fresh-keeping.It is fresh-keeping that chlorogenicacid is used for fruit juice, can effectively prevent the putrid and deteriorated of drink and food.In lard, if add a small amount of chlorogenicacid, can improve the lard oxidative stability, increase storage period.A small amount of chlorogenicacid is added in the natural solution, pigmentary colours are had stabilization, therefore, chlorogenicacid is again a kind of good foodstuff additive.Current, natural antioxidants more and more gets consumer reception, and chlorogenicacid is a kind of new and effective phenol type natural antioxidants, and instead or part replace present synthetic inhibitor in some food.
The chlorogenicacid purity difference that traditional technology is extracted will be carried through slightly carrying with essence repeatedly, causes extraction yield lower.
Summary of the invention:
The present invention is exactly to the problems referred to above, and the extraction process of chlorogenicacid in the Japanese Honeysuckle that a kind of extraction step is few, extraction yield is high is provided.
In order to realize above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and the present invention utilizes ethanol refluxing process that the former green acids in the Japanese Honeysuckle is extracted, and process step of the present invention is:
1. microwave treatment
The Japanese Honeysuckle of in the 250ml microwave special container of prolong is housed, packing into, the pre-soaking time is 8～24h, the setting microwave power is 600～800W, radiated time is 1～3min, starts microwave oven, extract finish after, united extraction liquid, concentrate drying obtains crude extract;
2. enzymolysis and extraction
In crude extract, add 0～3.0% enzymolysis solution, hydrolysis temperature is 25～60 ℃, and enzymolysis time is 1～4h; The adding solid-liquid ratio is 1: 8～1: 12 a ethanol, and concentration of ethanol is 65～75%, backflow lixiviate 0.5～1.5h;
3. the purifying of chlorogenicacid
The adding solid-liquid ratio is 1: 2～1: 5 a water in the chlorogenicacid crude extract, and deposition, the concentrate drying that filters, filtrates obtain finished product.
Beneficial effect of the present invention:
1. simple to operate, the energy-saving and environmental protection of the present invention;
2. chlorogenicacid yield of the present invention is 32.9%, is significantly increased than conventional method of extraction.
Embodiment:
Process step of the present invention is:
1. microwave treatment
The Japanese Honeysuckle of in the 250ml microwave special container of prolong is housed, packing into, the pre-soaking time is 8～24h, the setting microwave power is 600～800W, radiated time is 1～3min, starts microwave oven, extract finish after, united extraction liquid, concentrate drying obtains crude extract;
2. enzymolysis and extraction
In crude extract, add 0～3.0% enzymolysis solution, hydrolysis temperature is 25～60 ℃, and enzymolysis time is 1～4h; The adding solid-liquid ratio is 1: 8～1: 12 a ethanol, and concentration of ethanol is 65～75%, backflow lixiviate 0.5～1.5h;
3. the purifying of chlorogenicacid
The adding solid-liquid ratio is 1: 2～1: 5 a water in the chlorogenicacid crude extract, and deposition, the concentrate drying that filters, filtrates obtain finished product.
The present invention selects soak time, microwave irradiation time in the microwave process as the influence factor that influences the chlorogenicacid extraction yield, visible table 1, table 2.
The table 1 pre-soaking time is to the influence of chlorogenicacid extraction yield
| Pre-soaking time/h | 8 | 12 | 24 | 48 |
| Chlorogenicacid yield/% | 6.03 | 6.29 | 6.74 | 6.75 |
Table 2 microwave irradiation time is to the influence of chlorogenicacid extraction yield
| Radiated time/min | 1 | 2 | 3 |
| Chlorogenicacid yield/% | 6.24 | 6.73 | 6.74 |
As a kind of preferred version, process step of the present invention is: Japanese Honeysuckle pre-soaking 24h, microwave radiation 2min.
The present invention selects the consumption, enzymolysis time, hydrolysis temperature of enzyme as the factor that influences the chlorogenicacid extraction yield, visible table 3, table 4, table 5.
Table 3 enzyme dosage is to the influence of chlorogenicacid yield
| Enzyme dosage/ml | 0 | 0.5 | 1.0 | 1.5 | 2.0 | 2.5 | 3.0 |
| Chlorogenicacid yield/% | 5.75 | 5.84 | 6.12 | 6.46 | 6.67 | 6.69 | 6.73 |
Table 4 hydrolysis temperature is to the influence of chlorogenicacid yield
| Hydrolysis temperature | 25 | 30 | 35 | 40 | 45 | 50 | 55 | 60 |
| Chlorogenicacid yield/% | 5.95 | 6.27 | 6.63 | 7.18 | 7.36 | 7.15 | 6.59 | 6.11 |
Table 5 enzymolysis time is to the influence of chlorogenicacid yield
| Enzymolysis time/h | 1.0 | 1.5 | 2.0 | 2.5 | 3.0 | 3.5 | 4.0 |
| Chlorogenicacid yield/% | 6.25 | 6.58 | 6.94 | 7.28 | 7.46 | 7.48 | 7.51 |
As a kind of preferred version, process step of the present invention is: enzyme dosage is 2ml, and hydrolysis temperature is 40～50 ℃, and enzymolysis time is 3h.
The present invention selects alcohol concn, solid-liquid ratio, return time as the factor that influences the chlorogenicacid extraction yield, and as a kind of preferred version, process step of the present invention is: solid-liquid ratio is 1: 10, and alcohol concn is 75%, and extraction time is 1.5h.
Claims (4)
1. the extraction process of chlorogenicacid in the Japanese Honeysuckle is characterized in that, the present invention adopts following technical scheme, and the present invention utilizes ethanol refluxing process that the former green acids in the Japanese Honeysuckle is extracted, and process step of the present invention is:
(1) microwave treatment
The Japanese Honeysuckle of in the 250ml microwave special container of prolong is housed, packing into, the pre-soaking time is 8～24h, the setting microwave power is 600～800W, radiated time is 1～3min, starts microwave oven, extract finish after, united extraction liquid, concentrate drying obtains crude extract;
(2) enzymolysis and extraction
In crude extract, add 0～3.0% enzymolysis solution, hydrolysis temperature is 25～60 ℃, and enzymolysis time is 1～4h; The adding solid-liquid ratio is 1: 8～1: 12 a ethanol, and concentration of ethanol is 65～75%, backflow lixiviate 0.5～1.5h;
(3) purifying of chlorogenicacid
The adding solid-liquid ratio is 1: 2～1: 5 a water in the chlorogenicacid crude extract, and deposition, the concentrate drying that filters, filtrates obtain finished product.
2. the extraction process of chlorogenicacid is characterized in that in the Japanese Honeysuckle according to claim 1, and process step of the present invention is: Japanese Honeysuckle pre-soaking 24h, microwave radiation 2min.
3. the extraction process of chlorogenicacid is characterized in that in the Japanese Honeysuckle according to claim 1, and process step of the present invention is: enzyme dosage is 2ml, and hydrolysis temperature is 40～50 ℃, and enzymolysis time is 3h.
4. the extraction process of chlorogenicacid is characterized in that in the Japanese Honeysuckle according to claim 1, and process step of the present invention is: solid-liquid ratio is 1: 10, and alcohol concn is 75%, and extraction time is 1.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105522546A CN102476996A (en) | 2010-11-22 | 2010-11-22 | Extraction process of chlorogenic acid in honeysuckle |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105522546A CN102476996A (en) | 2010-11-22 | 2010-11-22 | Extraction process of chlorogenic acid in honeysuckle |
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| CN102476996A true CN102476996A (en) | 2012-05-30 |
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| CN2010105522546A Pending CN102476996A (en) | 2010-11-22 | 2010-11-22 | Extraction process of chlorogenic acid in honeysuckle |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911055A (en) * | 2012-11-13 | 2013-02-06 | 西南大学 | Method for extracting chlorogenic acid |
| CN103086889A (en) * | 2013-02-22 | 2013-05-08 | 王星敏 | Method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme |
| CN103864617A (en) * | 2012-12-07 | 2014-06-18 | 廉吉芳 | Method for extracting chlorogenic acid from honeysuckle |
| RU2589820C1 (en) * | 2015-05-29 | 2016-07-10 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Method for complex extraction of biologically active substances from medicinal plant raw materials on cellular level |
| CN106608822A (en) * | 2015-10-26 | 2017-05-03 | 恩施州地壹嘉知识产权服务有限公司 | Method for extracting chlorogenic acid from Laifeng crossostepium leaves |
| CN114031498A (en) * | 2021-11-05 | 2022-02-11 | 临沂市农业科学院 | Method for extracting high-purity honeysuckle chlorogenic acid by membrane separation method |
-
2010
- 2010-11-22 CN CN2010105522546A patent/CN102476996A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911055A (en) * | 2012-11-13 | 2013-02-06 | 西南大学 | Method for extracting chlorogenic acid |
| CN102911055B (en) * | 2012-11-13 | 2014-07-09 | 西南大学 | Method for extracting chlorogenic acid |
| CN103864617A (en) * | 2012-12-07 | 2014-06-18 | 廉吉芳 | Method for extracting chlorogenic acid from honeysuckle |
| CN103864617B (en) * | 2012-12-07 | 2016-04-06 | 廉吉芳 | A kind of method of chlorogenic acid extracting from Japanese Honeysuckle |
| CN103086889A (en) * | 2013-02-22 | 2013-05-08 | 王星敏 | Method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme |
| CN103086889B (en) * | 2013-02-22 | 2015-11-25 | 王星敏 | A kind of method of enzyme catalysis activation leaf of Flos Lonicerae chlorogenic acid extracting |
| RU2589820C1 (en) * | 2015-05-29 | 2016-07-10 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Method for complex extraction of biologically active substances from medicinal plant raw materials on cellular level |
| CN106608822A (en) * | 2015-10-26 | 2017-05-03 | 恩施州地壹嘉知识产权服务有限公司 | Method for extracting chlorogenic acid from Laifeng crossostepium leaves |
| CN106608822B (en) * | 2015-10-26 | 2021-02-02 | 恩施州地壹嘉知识产权服务有限公司 | Method for extracting chlorogenic acid from Dendranthema indicum |
| CN114031498A (en) * | 2021-11-05 | 2022-02-11 | 临沂市农业科学院 | Method for extracting high-purity honeysuckle chlorogenic acid by membrane separation method |
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Application publication date: 20120530 |