CN102824431A - Method for extracting hawthorn flavone by using pressurized liquid extraction (APLE) technique - Google Patents
Method for extracting hawthorn flavone by using pressurized liquid extraction (APLE) technique Download PDFInfo
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- CN102824431A CN102824431A CN2012103255588A CN201210325558A CN102824431A CN 102824431 A CN102824431 A CN 102824431A CN 2012103255588 A CN2012103255588 A CN 2012103255588A CN 201210325558 A CN201210325558 A CN 201210325558A CN 102824431 A CN102824431 A CN 102824431A
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Abstract
The invention discloses a method for extracting flavone component in hawthorn by using a pressurized liquid extraction (APLE) technique. The method comprises removing kernels from matured hawthorn fruits, conducting low-temperature drying, smashing by using a grinder, screening hawthorn powder with needed particle size, placing for reserving, weighting certain amount of the hawthorn powder to be sufficiently mixed with certain amount of kieselguhr, filling in an extraction pool, sealing the extraction pool, placing in a pressurized solvent extraction device, adding solvent, setting parameters and then automatically extracting. Maximum 12 samples can be automatically extracted by using a same method. The pressurized liquid extraction method is adopted, extracting time is short, conditions are mild, the solvent is saved, and flavone yield is high. The method further has the advantages of simple operation, good continuity and the like. Obtained hawthorn flavone can be used for further research and development of medical treatment, health care and functional foods.
Description
Technical field
The invention belongs to natural product extracting technique, relate to a kind of technology of utilizing pressurized liquid extraction (APLE) method to extract flavonoid substance in the Fructus Crataegi specifically.
Background technology
The raw material haw berry, Rosaceae Crataegus, but medicine-food two-purpose, abundant in china natural resources.Compendium of Material Medica notebook article " sour sweet tepor, it is long-pending to help digestion, spleen reinforcing ".Fructus Crataegi is warm in nature, sour in the mouth, have the effect of promoting digestion and removing stagnation, blood circulation promoting and blood stasis dispelling, and the clinical fruit that mainly is dried is used for food stagnation, women's postpartum stagnation stomachache, hernia, children's's varioliform exanthema etc.The Fructus Crataegi The Chemical Constituents is started from nineteen twenty-one; Research before the 1950's; Focus mostly at compositions such as its contained cellulose, tannin, triterpeness; Along with the developing rapidly of flavone compound, find that contained flavones ingredient has tangible pharmacological action to cardiovascular system in the Fructus Crataegi after the fifties, research emphasis turns to flavones ingredient.
The pressurized liquid extraction technology is a kind of new method that is proposed by (1995) such as Richter.Be recommended as a kind of extracting process of standard by American National Environmental Protection Agency (EPA).The pressurized liquid extraction technology is the new technique that just developed in recent years, because it is with conspicuous characteristics, has received the very big concern of analytical chemistry circle.This technology is used widely in fields such as environment, medicine, food, agricultural and polymer industry.Utilize the pressurized liquid extraction technology that the method that flavonoid substance in the Fructus Crataegi extracts is not seen relevant report at present as yet.
Summary of the invention
The purpose of this invention is to provide a kind of technology of utilizing the pressurized liquid extraction method to extract flavonoid substance in the Fructus Crataegi.Have that solvent load is few, simple to operate, the time spent is short, the extraction efficiency advantages of higher.Simultaneously, because its extraction conditions is gentle, kept the biological activity of flavonoid substance.
Method for distilling of the present invention comprises:
1, get the period of maturation Fructus Crataegi, after the enucleation, carry out 5 ℃-25 ℃ of cold drying, pulverize, the Fructus Crataegi powder after pulverizing is packed into behind the sealing bag, put into exsiccator with pulverizer, subsequent use;
2, it is even by the 1:1-1.5 mixed to get above-mentioned dry Fructus Crataegi powder and kieselguhr, adds in the abstraction pool, adds an amount of kieselguhr again and fills the abstraction pool space, and the sealing abstraction pool is placed on the abstraction instrument opposite position with abstraction pool and receiving flask, the access extractant;
3, open the nitrogen steel cylinder, regulating nitrogen partial pressure is 0.8 MPa-1 MPa, opens the abstraction instrument power supply, and the abstraction instrument self check is cleaned the abstraction instrument pipeline with cleaning solvent after self check is accomplished, and sets 40 ℃-120 ℃ beginnings of preheat temperature preheating;
4, after step 3 is accomplished, extraction conditions is set: 40 ℃-120 ℃ of extraction temperature, heat time heating times 3 min-15 min; Extraction pressure: 3 MPa-15 MPa, cycle-index: 1-5 time, elution volume 40 %-60 %; Nitrogen blows time 40-100 s, and extraction obtains the Fructus Crataegi flavone crude extract after accomplishing.
In the present invention, described extractant and cleaning solvent are methanol, ethanol, or the mixed solution of second alcohol and water.
Remarkable advantage of the present invention:
The present invention adopts pressurized liquid extraction (APLE) technology to extract Fructus Crataegi flavone.Compare existing other method for distilling, have extraction time weak point, practice thrift reagent, reacting balance, the flavone yield is high, the outstanding advantage that simple to operate, seriality is good.Simultaneously health environment-friendly, automaticity are high, have kept the biological activity of flavonoid substance.
The specific embodiment
Embodiment 1
1, get ripe Fructus Crataegi, after enucleation, cold drying, baking temperature is 15 ℃-25 ℃, pulverizes with pulverizer, in the sealing bag of packing into, it is subsequent use to put into exsiccator;
2, accurately take by weighing 25 g Fructus Crataegi powder and 20 g kieselguhr mix homogeneously, in the 100mL abstraction pool of packing into, the sealing abstraction pool is placed the abstraction instrument opposite position with abstraction pool and receiving flask, inserts 50% ethanol;
3, open the nitrogen valve, regulating nitrogen partial pressure is 0.8 MPa, opens the abstraction instrument power supply, instrument self checking, and the ethanol with 50% after self check is accomplished cleans the abstraction instrument pipeline, sets 50 ℃ of beginnings of preheat temperature preheating;
4, after step 3 is accomplished, extraction conditions is set: 50 ℃ of extraction temperature, extraction times 4 min, extraction pressure: 10 MPa, cycle-index: 1, elution volume 60 %, nitrogen blows times 60 s, and extraction obtains the Fructus Crataegi flavone crude extract after accomplishing.
Embodiment 2
1, adopt the step 1 of embodiment 1 to handle subsequent use equally;
2, accurately take by weighing 20 g Fructus Crataegi powder and 20 g kieselguhr mix homogeneously, in the 100mL abstraction pool of packing into, add 5 g kieselguhr blinds again, the sealing abstraction pool puts abstraction pool and receiving flask to the abstraction instrument relative position, inserts methanol;
3, open the nitrogen valve, regulating nitrogen partial pressure is 0.8 MPa, opens the abstraction instrument power supply, and instrument self checking with washed with methanol abstraction instrument pipeline, is set 60 ℃ of beginnings of preheat temperature preheating after self check is accomplished;
4, after step 3 is accomplished, extraction conditions is set: 60 ℃ of extraction temperature, extraction times 8 min, extraction pressure: 10 MPa, cycle-index: 2, elution volume 60 %, nitrogen blows times 60 s, and extraction obtains the Fructus Crataegi flavone crude extract after accomplishing.
Embodiment 3
1, adopt the step 1 of embodiment 1 to handle subsequent use equally;
2, get dry Fructus Crataegi powder 30 g and the abundant mix homogeneously of kieselguhr 15 g of above-mentioned processing; Pack in the abstraction pool, and then add 5 g kieselguhr and fill up abstraction pool, connect nitrogen device and abstraction instrument; Abstraction pool and receiving flask are placed on the abstraction instrument opposite position, insert 70% ethanol;
3, open the nitrogen valve, regulating nitrogen partial pressure is 0.8 MPa, opens the abstraction instrument power supply, and instrument self checking cleans the abstraction instrument pipeline with 70% ethanol after self check is accomplished, and sets 70 ℃ of beginnings of preheat temperature preheating;
4, after step 3 is accomplished, extraction conditions is set: 70 ℃ of extraction temperature, extraction times 12 min, extraction pressure: 10 MPa, cycle-index: 3, elution volume 60 %, nitrogen blows times 60 s, and extraction obtains the Fructus Crataegi flavone crude extract after accomplishing.
Embodiment 4
1, adopt the step 1 of embodiment 1 to handle subsequent use equally;
2, get dry Fructus Crataegi powder 20 g and the abundant mix homogeneously of kieselguhr 30 g of above-mentioned processing; Pack in the abstraction pool, and then add 5 g kieselguhr and fill up abstraction pool, connect nitrogen device and abstraction instrument; Abstraction pool and receiving flask are placed on the abstraction instrument opposite position, insert dehydrated alcohol;
3, open the nitrogen valve, regulating nitrogen partial pressure is 0.8 MPa, opens the abstraction instrument power supply, and instrument self checking cleans the abstraction instrument pipeline with dehydrated alcohol after self check is accomplished, and sets 70 ℃ of beginnings of preheat temperature preheating;
4, behind the completing steps 3, extraction conditions is set: 70 ℃ of extraction temperature, extraction times 4 min, extraction pressure: 10 MPa, cycle-index: 3, elution volume 60 %, nitrogen blows times 60 s, and extraction obtains the Fructus Crataegi flavone crude extract after accomplishing.
The foregoing description only is used for the reference as technical scheme of the present invention, not as the single restrictive condition of technical scheme itself.
Claims (2)
1. one kind is utilized the technological method of extracting Fructus Crataegi flavone of pressurized liquid extraction (APLE), and its method comprises:
(1) get the period of maturation Fructus Crataegi, after the enucleation, carry out 5 ℃-25 ℃ of cold drying, pulverize, behind the sealing bag of packing into, put into exsiccator, subsequent use;
(2) it is even by the 1:1-1.5 mixed to get above-mentioned dry Fructus Crataegi powder and kieselguhr, adds in the abstraction pool, adds an amount of kieselguhr again and fills the abstraction pool space, and abstraction pool and receiving flask are placed on the abstraction instrument opposite position, the access extractant;
(3) open the nitrogen steel cylinder, regulating nitrogen partial pressure is 0.8 MPa-1 MPa, opens the abstraction instrument power supply, and the abstraction instrument self check is cleaned the abstraction instrument pipeline with cleaning solvent after self check is accomplished, and sets 40 ℃-120 ℃ beginnings of preheat temperature preheating;
(4) after step 3 is accomplished, extraction conditions is set: 40 ℃-120 ℃ of extraction temperature, extraction times 3 min-15 min; Extraction pressure: 3 MPa-15 MPa, cycle-index: 1-5 time, elution volume 40 %-60 %; Nitrogen blows time 40-100 s, and extraction obtains the Fructus Crataegi flavone crude extract after accomplishing.
2. the extraction process of Fructus Crataegi flavone according to claim 1, it is characterized in that: wherein extractant and cleaning solvent are ethanol, methanol, or the mixed solution of second alcohol and water.
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| CN2012103255588A CN102824431A (en) | 2012-09-06 | 2012-09-06 | Method for extracting hawthorn flavone by using pressurized liquid extraction (APLE) technique |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103142721A (en) * | 2013-03-15 | 2013-06-12 | 河北科技师范学院 | Method for extracting triterpenoid from anli pear |
| CN104126782A (en) * | 2014-07-29 | 2014-11-05 | 桂林实力科技有限公司 | Grosvenor momordica sweetener and preparation method thereof |
| CN106238000A (en) * | 2016-08-09 | 2016-12-21 | 长安大学 | A kind of Folium Bambosae flavone cellulose adsorbent, preparation method and applications |
| CN109966773A (en) * | 2017-11-22 | 2019-07-05 | 大江生医股份有限公司 | The method of active constituent is extracted from object to be extracted |
| CN111772187A (en) * | 2020-07-02 | 2020-10-16 | 吕剑 | Sour carambola extract, extraction method thereof and product thereof |
| CN112691046A (en) * | 2021-01-09 | 2021-04-23 | 陈健 | Hawthorn extract neck wrinkle cream and preparation method thereof |
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| CN102539572A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence |
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| CN102539572A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence |
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| 张玉等: "加速溶剂萃取技术提取柑橘皮中总黄酮的工艺研究", 《食品科技》, no. 11, 31 December 2007 (2007-12-31), pages 215 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103142721A (en) * | 2013-03-15 | 2013-06-12 | 河北科技师范学院 | Method for extracting triterpenoid from anli pear |
| CN104126782A (en) * | 2014-07-29 | 2014-11-05 | 桂林实力科技有限公司 | Grosvenor momordica sweetener and preparation method thereof |
| CN104126782B (en) * | 2014-07-29 | 2015-10-21 | 桂林实力科技有限公司 | A kind of momordica grosvenori sweetening agent and preparation method thereof |
| CN106238000A (en) * | 2016-08-09 | 2016-12-21 | 长安大学 | A kind of Folium Bambosae flavone cellulose adsorbent, preparation method and applications |
| CN106238000B (en) * | 2016-08-09 | 2018-12-28 | 长安大学 | A kind of bamboo-leaves flavones cellulose adsorbent, preparation method and applications |
| CN109966773A (en) * | 2017-11-22 | 2019-07-05 | 大江生医股份有限公司 | The method of active constituent is extracted from object to be extracted |
| CN111772187A (en) * | 2020-07-02 | 2020-10-16 | 吕剑 | Sour carambola extract, extraction method thereof and product thereof |
| CN111772187B (en) * | 2020-07-02 | 2023-04-07 | 吕剑 | Sour carambola extract, extraction method thereof and product thereof |
| CN112691046A (en) * | 2021-01-09 | 2021-04-23 | 陈健 | Hawthorn extract neck wrinkle cream and preparation method thereof |
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Application publication date: 20121219 |