CN104004036A - Extraction technology of honeysuckle flower galuteolin - Google Patents

Extraction technology of honeysuckle flower galuteolin Download PDF

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Publication number
CN104004036A
CN104004036A CN201410166152.9A CN201410166152A CN104004036A CN 104004036 A CN104004036 A CN 104004036A CN 201410166152 A CN201410166152 A CN 201410166152A CN 104004036 A CN104004036 A CN 104004036A
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China
Prior art keywords
galuteolin
ethanol
luteolin
carrying
honeysuckle
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CN201410166152.9A
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Chinese (zh)
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王正鹏
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Liuyang City Heng Ji Agricultural Development Co Ltd
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Liuyang City Heng Ji Agricultural Development Co Ltd
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Priority to CN201410166152.9A priority Critical patent/CN104004036A/en
Publication of CN104004036A publication Critical patent/CN104004036A/en
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Abstract

The invention relates to the technical field of intensive processing of honeysuckle flower, and especially relates to an extraction technology of honeysuckle flower galuteolin. The technology comprises the following steps: 1, drying; 2, crushing, adding ethanol, heating, carrying out reflux extraction, and carrying out press filtration to obtain an extract liquid; 3, adding ethanol with the concentration of 75% to filter residues, and carrying out press filtration to obtain an extract liquid; 4, mixing the extract liquid obtained in step 2 with the extract liquid obtained in step 3, and concentrating the obtained filtrate to form a syupy substance; 5, carrying out macroporous resin adsorption on the obtained concentrate, and eluting with ethanol to obtain crude galuteolin; 6, repeating step 5 to obtain refined galuteolin; 7, carrying out reduced pressure distillation to recover ethanol; 8, cooling raffinate to 4DEG C, and allowing the cooled raffinate to stand for 48h in order to obtain galuteolin crystals with the purity of 95.8-98%; and 8, carrying out vacuum drying on the crystals. The technology has the advantages of provision of a stable selling market for peasants, protection of the benefit of the peasants, effective increase of the income of the peasants, full utilization of the agriculture resource, improvement of the added values of agricultural products and enhancement of the market competitiveness of the agricultural products by exploiting intensive processing products of honeysuckle flower.

Description

A kind of extraction process of Japanese Honeysuckle galuteolin
Technical field
The present invention relates to Japanese Honeysuckle intensive processing technical field, refer to especially a kind of extraction process of Japanese Honeysuckle galuteolin.
Background technology
Along with improving constantly of living standards of the people, people to life pursuit by simply having adequate food and clothing to mass type and health future development, Japanese Honeysuckle healthcare products series product, there is resisting pathogenic microbes, enhancing immunologic function, clearing heat and detoxicating, the medicinal efficacies such as depreciation step-down of losing weight, hypertension, obesity, cancer, SARS etc. are had and prevent and treat preferably function, liked by human consumer.
According to crude drug source and the medicinal material title of < < Chinese Pharmacopoeia > > 2005 version (part), using Japanese Honeysuckle as Japanese Honeysuckle and two kinds of medicinal materials of Lonicera confusa DC. include, it is a kind of that Japanese Honeysuckle has only been included honeysuckle, and crude drug source using largeflower-like honeysuckle flower, lonicera hypoglauca miq, Lonicera confusa as Lonicera confusa DC..Major cause is that Japanese Honeysuckle galuteolin content is high.According to pharmacological experiments, galuteolin has stronger respiratory tract germicidal action, reduces the effect of cholesterol in atherosclerosis, strengthens the diastole effect of capillary vessel.Therefore,, in clinical formulation and in Chinese patent medicine production, according to the effect of prescription, select suitable crude drug source and plant origin.The standard of version < < Chinese Pharmacopoeia > > regulation traditional Chinese medicine honeysuckle in 2005 is: containing chlorogenic acid, must not be less than 1.5%, containing galuteolin, must not be less than 0.1%.According to the chlorogenic acid content of measuring largeflower-like honeysuckle flower between 3%-7%, far away higher than national standard.Galuteolin content between 0.1%-0.15%, also meet that < < Chinese Pharmacopoeia > > works out honeysuckle medicinal material standard.
Summary of the invention
The object of the present invention is to provide a kind of extraction process of Japanese Honeysuckle galuteolin,
Technical scheme of the present invention comprises the following steps: a. extracting honeysuckle is put 60 ℃ of oven drying 12h; B. by dry Japanese Honeysuckle crushing material to 20 to 40 orders, by 6 to 10 times of weight of material, add concentration 75 to 85% ethanol, be heated to 60 to 80 ℃, refluxing extraction 1 is to 3h, in 0.5 to 0.7Mpa pressure range, press filtration obtains extracting solution; C. filter residue adds the extraction using alcohol 0.5 of concentration 75% to 1.5h by 8 to 10 times of weight of material, and in 0.5 to 0.7Mpa pressure range, press filtration obtains extracting solution; D. merging filtrate, is decompressed to 0.05 to 0.07Mpa, and concentrated filtrate is to syrupy shape; E. concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin; F. repeating step e is mono-to three time, obtains luteolin essence product; G. be incorporated in isopyknic 60 to the 80 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation; H. after remaining liquid cooling but to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%; I. crystallization vacuum-drying.
The step f gained luteolin essence product also activated carbon decolorizing of 1 to 3 times of available filtrate weight enters step g again.
Step h repeats to enter step I one to three time.
The invention has the advantages that, exploitation Japanese Honeysuckle deep processed product, not only can provide a stable selling market for peasant; protection peasant's interests, effectively increase farmers' income, and can also make full use of agricultural resource; improve agricultural product added value, strengthen the market competitiveness of agricultural-food.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described,
Embodiment mono-comprises the following steps: a. extracting honeysuckle is put 60 ℃ of oven drying 12h; B. by dry Japanese Honeysuckle crushing material to 40 order, by 10 times of weight of material, add concentration 85% ethanol, be heated to 80 ℃, refluxing extraction 1 h, in the pressure range of 0.7Mpa, press filtration obtains extracting solution; C. filter residue is by 8 times of the weight of material extraction using alcohol 0.5h that add concentration 75%, and in the pressure range of 0.5 Mpa, press filtration obtains extracting solution; D. merging filtrate, is decompressed to 0.07Mpa, and concentrated filtrate is to syrupy shape; E. concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin; F. repeating step e is tri-times, obtains luteolin essence product; G. be incorporated in the isopyknic 80 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation; H. after remaining liquid cooling but to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%; I. crystallization vacuum-drying.
The step f gained luteolin essence product also activated carbon decolorizing of 3 times of available filtrate weight enters step g again.
Step h repeats once to enter step I.
Embodiment bis-comprises the following steps: a. extracting honeysuckle is put 60 ℃ of oven drying 12h; B. by dry Japanese Honeysuckle crushing material to 20 order, by 6 times of weight of material, add concentration 75 % ethanol, be heated to 60 ℃, refluxing extraction 3h, in the pressure range of 0.6Mpa, press filtration obtains extracting solution; C. filter residue is by 8 times of the weight of material extraction using alcohol 1.5h that add concentration 75%, and in the pressure range of 0.6Mpa, press filtration obtains extracting solution; D. merging filtrate, is decompressed to 0.06Mpa, and concentrated filtrate is to syrupy shape; E. concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin; F. repeating step e once, obtains luteolin essence product; G. be incorporated in the isopyknic 60 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation; H. after remaining liquid cooling but to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%; I. crystallization vacuum-drying.
The step f gained luteolin essence product also activated carbon decolorizing of 1 times of available filtrate weight enters step g again.
Step h enters step I in triplicate.
Embodiment tri-comprises the following steps: a. extracting honeysuckle is put 60 ℃ of oven drying 12h; B. by dry Japanese Honeysuckle crushing material to 30 order, by 80 times of weight of material, add concentration 80% ethanol, be heated to 70 ℃, refluxing extraction 2h, in the pressure range of 0.7Mpa, press filtration obtains extracting solution; C. filter residue is by 10 times of the weight of material extraction using alcohol 0.5h that add concentration 75%, and in the pressure range of 0.5 Mpa, press filtration obtains extracting solution; D. merging filtrate, is decompressed to 0.07Mpa, and concentrated filtrate is to syrupy shape; E. concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin; F. repeating step e is bis-times, obtains luteolin essence product; G. be incorporated in the isopyknic 80 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation; H. after remaining liquid cooling but to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%; I. crystallization vacuum-drying.
The step f gained luteolin essence product also activated carbon decolorizing of 2 times of available filtrate weight enters step g again.
Step h repeats secondary and enters step I.
Embodiment tetra-comprises the following steps: a. extracting honeysuckle is put 60 ℃ of oven drying 12h; B. by dry Japanese Honeysuckle crushing material to 25 order, by 7 times of weight of material, add concentration 75% ethanol, be heated to 65 ℃, refluxing extraction 3h, in the pressure range of 0.5 Mpa, press filtration obtains extracting solution; C. filter residue is by 9 times of the weight of material extraction using alcohol 1h that add concentration 75%, and in the pressure range of 0.5 Mpa, press filtration obtains extracting solution; D. merging filtrate, is decompressed to 0.07Mpa, and concentrated filtrate is to syrupy shape; E. concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin; F. repeating step e once, obtains luteolin essence product; G. be incorporated in the isopyknic 60 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation; H. after remaining liquid cooling but to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%; I. crystallization vacuum-drying.
The step f gained luteolin essence product also activated carbon decolorizing of 3 times of available filtrate weight enters step g again.
Step h enters step I in triplicate.
Embodiment five comprises the following steps: a. extracting honeysuckle is put 60 ℃ of oven drying 12h; B. by dry Japanese Honeysuckle crushing material to 35 order, by 7 times of weight of material, add concentration 75 % ethanol, be heated to 60 ℃, refluxing extraction 1.5h, in the pressure range of 0.6Mpa, press filtration obtains extracting solution; C. filter residue is by 10 times of the weight of material extraction using alcohol 1h that add concentration 75%, and in the pressure range of 0.5 Mpa, press filtration obtains extracting solution; D. merging filtrate, is decompressed to 0.07Mpa, and concentrated filtrate is to syrupy shape; E. concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin; F. repeating step e once, obtains luteolin essence product; G. be incorporated in the isopyknic 60 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation; H. after remaining liquid cooling but to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%; I. crystallization vacuum-drying.
The step f gained luteolin essence product also activated carbon decolorizing of 1 times of available filtrate weight enters step g again.
Step h repeats once to enter step I.

Claims (3)

1. an extraction process for Japanese Honeysuckle galuteolin, its feature comprises the following steps:
A .extracting honeysuckle is put 60 ℃ of oven drying 12h;
B .dry Japanese Honeysuckle crushing material to 20, to 40 orders, is added to concentration 75 to 85% ethanol by 6 to 10 times of weight of material, be heated to 60 to 80 ℃, refluxing extraction 1 is to 3h, and in 0.5 to 0.7Mpa pressure range, press filtration obtains extracting solution;
C .filter residue adds the extraction using alcohol 0.5 of concentration 75% to 1.5h by 8 to 10 times of weight of material, and in 0.5 to 0.7Mpa pressure range, press filtration obtains extracting solution;
D .merging filtrate, is decompressed to 0.05 to 0.07Mpa, and concentrated filtrate is to syrupy shape;
E .concentrated solution macroporous resin adsorption, the ethanol elution by concentration 75%, obtains the thick product of luteolin;
F. repeating step e is mono-to three time, obtains luteolin essence product;
G .be incorporated in isopyknic 60 to the 80 ℃ of hot water of ethanol, ethanol is reclaimed in underpressure distillation;
H .after remaining liquid cooling but, to standing 48h at 4 ℃, obtain the luteolin crystallization of purity 95.8 to 98%;
I .crystallization vacuum-drying.
2. the extraction process of a kind of Japanese Honeysuckle galuteolin according to claim 1, it is characterized in that step f gained luteolin essence product also the activated carbon decolorizing of 1 to 3 times of available filtrate weight enter again step g.
3. the extraction process of a kind of Japanese Honeysuckle galuteolin according to claim 1, is characterized in that step h repeats to enter step I one to three time.
CN201410166152.9A 2014-04-24 2014-04-24 Extraction technology of honeysuckle flower galuteolin Pending CN104004036A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105175464A (en) * 2015-06-17 2015-12-23 广东省农业科学院蚕业与农产品加工研究所 Method for separating luteolin 5-O-beta-glucoside from dried longan pulp
CN105622655A (en) * 2016-01-14 2016-06-01 临沂大学 Rare earth-luteolin-imidazole ternary complex and preparation method thereof
CN105646424A (en) * 2014-11-15 2016-06-08 北京农学院 A method of extracting luteolin
CN107337660A (en) * 2017-07-24 2017-11-10 仲恺农业工程学院 The extracting method of cyanidenon in a kind of honeysuckle
CN108892694A (en) * 2018-09-16 2018-11-27 湖州展舒生物科技有限公司 The preparation method of galuteolin

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105646424A (en) * 2014-11-15 2016-06-08 北京农学院 A method of extracting luteolin
CN105646424B (en) * 2014-11-15 2017-12-05 北京农学院 A kind of method for extracting cyanidenon
CN105175464A (en) * 2015-06-17 2015-12-23 广东省农业科学院蚕业与农产品加工研究所 Method for separating luteolin 5-O-beta-glucoside from dried longan pulp
CN105175464B (en) * 2015-06-17 2018-03-20 广东省农业科学院蚕业与农产品加工研究所 The method that the O β glucosides of cyanidenon 5 are separated from arillus longan
CN105622655A (en) * 2016-01-14 2016-06-01 临沂大学 Rare earth-luteolin-imidazole ternary complex and preparation method thereof
CN107337660A (en) * 2017-07-24 2017-11-10 仲恺农业工程学院 The extracting method of cyanidenon in a kind of honeysuckle
CN108892694A (en) * 2018-09-16 2018-11-27 湖州展舒生物科技有限公司 The preparation method of galuteolin

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Application publication date: 20140827