CN105384716A - Method for enriching and purifying lycium ruthenicum Murr anthocyanin - Google Patents
Method for enriching and purifying lycium ruthenicum Murr anthocyanin Download PDFInfo
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- CN105384716A CN105384716A CN201510761428.2A CN201510761428A CN105384716A CN 105384716 A CN105384716 A CN 105384716A CN 201510761428 A CN201510761428 A CN 201510761428A CN 105384716 A CN105384716 A CN 105384716A
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- matrimony vine
- black matrimony
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- anthocyanidin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the field of natural organic chemistry and relates to a method for purifying lycium ruthenicum Murr anthocyanin and in particular relates to a method for purifying the lycium ruthenicum Murr anthocyanin by utilizing the macroporous resin technology. The method has the beneficial effects that inorganic acid is used as an extracting solution and extraction is carried out complete; the production efficiency is improved; the method is simple; the macroporous resin is convenient and fast to regenerate and is suitable for large-scale production; the cost is greatly reduced; most impurities are removed through elution with water and the operation is easy to carry out; meanwhile, the content of active ingredients is increased.
Description
Technical field
The present invention relates to a kind of extracting method of black matrimony vine anthocyanidin, particularly relate to the method utilizing acid extraction black structure Qi anthocyanidin.
Background technology
Wild black matrimony vine, also known as black fruit lyceum, covers Qiao Nuoyinghaer mug(unit of measure) by name, the other agate black fruit lyceum of Tibetan medicine name; Taste is sweet, property is flat, the multiple nutritional components such as rich in proteins, lycium barbarum polysaccharide, amino acid, VITAMIN, mineral substance, trace element; Also containing abundant black fruit pigment natural procyanidins; Black fruit lyceum is containing OPC3690mg/100g, and blueberry is the wild plant finding that OPC content is the highest up to now containing OPC330 ~ 3380mg/100g.Pycnogenols OPC is the most effective water-soluble free-radical scavengers, and its effect is 20 times of Vc, 50 times of VE, and black matrimony vine is described as a wild blueness goblin Ji.
The wild black fruit lyceum adaptability of habit of wild black fruit lyceum is very strong, can restrain oneself 38.5 celsius temperatures, and winter hardiness is also very strong, without freeze injury under-25.6 degrees Celsius, drought-resistant, still can grow on desert ground.Be intolerant tree species, grow healthy and strong under full exposure, giving shade, lower growth is thin and delicate, and flowers and fruits are few.Require not tight to soil, its background soil 0 ~ 10cm soil layer soil salt content can reach 8.9%, and 10 ~ 30cm soil layer soil salt content can reach 5.1%, and Rhizosphere Soil soil salt content reaches 2.5%, as seen its Salt And Alkali Tolerance ability extra-heavy, and has stronger suction salt ability; Waterlogging-resistant ability, low-lying water accumulation part should not be planted.Many happinesses are born in the various salinification habitat soils such as saline-alkali wasteland, salinization sand ground, bank, salt lake, Qu Lu both sides, river shoal.
Northwest Plateau-organisms Research Inst. of Chinese Academy of Sciences, Postgraduate School, Chinese Academy of Sciences analyze the main nutrient composition in the wild black Chinese wolfberry fruit in excellent Yi Tang Qaidam, result shows, black medlar fresh fruit water content 85.03%, its dry fruit protein mass mark 10.61%, fat 6.66%, polysaccharide 4.28%, total flavones massfraction 4.29%, pycnogenols 3.42%.Fruit contains γ-VE and δ-VE, every hectogram is respectively 0.0075 and 0.016mg, the Boxthorn Seed Oil content of vitamin E extracted from black matrimony vine seed is much higher compared with fruit, and seed oil is rich in α-VE, γ-VE and δ-VE, and every hectogram is respectively 0.1906mg, 1.8939mg and 0.045mg.In black matrimony vine, amino acid classes is relatively abundant, and leucine, methionine(Met), phenylalanine, Isoleucine equal size are relatively high.Black matrimony vine Mineral Elements enriches, and wherein the content of potassium is the highest, and far above the content of sodium, belongs to the food of hyperkalemia hyponatremia.Trace element simultaneously contained by fruit is also very abundant, except major element Na, K, Mg, Ca, Fe, also containing a certain amount of micro-Mn, Sr, Se, Zn, Cr, Cu etc.Because trace element is to the synthesis of the activity of multiple enzyme and nucleic acid, protein, immunity of organism and cell proliferation etc. have and act on directly or indirectly, can be used for cancer preventing and treating.
Summary of the invention
The object of the present invention is to provide the method utilizing the black matrimony vine anthocyanidin of acid extraction, the method, compared with conventional extraction, substantially reduces extraction time, and product yield is high, and cost is low, is convenient to produce.
The invention provides a kind of method utilizing anthocyanidin in the black matrimony vine of acid extraction enriching and purifying, its step comprises:
(1) black matrimony vine is broken, sieving, is that the inorganic acid aqueous solution of 0.3% ~ 0.7% mixes respectively with concentration, solid-liquid ratio is 1: 8 ~ 1: 10, regulates pH value 1.0 ~ 2.0, carries out insulation and extracts, the temperature that insulation is extracted, at 50 ~ 60 DEG C, is extracted 2 ~ 3 hours, filters.
(2) gained filtered liquid carries out underpressure distillation, and pressure-controlling is at 0.1 ~ 0.2Mpa, and temperature controls at 50 ~ 60 DEG C.
(3) filtered liquid is through macroporous resin adsorption to saturated, and macroporous resin model is the one in HPD400, DM-130, AB-8 and NKA-II type resin, and the aspect ratio of resin column is 8: 1-15: 1, is adsorbed as Static Adsorption or dynamic adsorption.
(4) at normal temperatures and pressures, with 1BV/h flow velocity, first use distilled water wash-out, elution volume is 3-5BV, washes the water-soluble impurity in the black matrimony vine aqueous solution off.
(5) with the ethanol of 70% ~ 90% concentration, elution volume is carry out wash-out under 6-8BV, uses tlc tracing detection, collects each stepwise elution liquid of the black matrimony vine aqueous solution.
(6) elutriant is at pressure-0.07 ~ 0.08Mpa, and under 50 ~ 60 DEG C of conditions, through decompression recycling ethanol, obtain black matrimony vine concentrated solution, its proportion is 1.08 ~ 1.12.
(7) concentrated solution carries out vacuum-drying at 70 ~ 80 DEG C, and obtain black matrimony vine anthocyanidin finished product, moisture controlled is below 5%, and its content is more than 25%.
The present invention is using mineral acid as extraction solution, and extract completely, improve production efficiency, method is simple.Macroporous resin regeneration is rapidly convenient, and be applicable to large production, and cost reduces greatly, water elution removes most of impurity, easily operates; Improve active constituent content simultaneously.
Embodiment:
Embodiment 1: the invention provides a kind of method utilizing anthocyanidin in the black matrimony vine of acid extraction enriching and purifying, its step comprises:
(1) black matrimony vine is broken, cross 60 mesh sieves, the inorganic acid aqueous solution being 0.3% with concentration mixes, and solid-liquid ratio is 1: 8, regulates pH value 1.5, and carry out insulation and extract, the temperature that insulation is extracted, at 60 DEG C, is extracted 3 hours, filters.
(2) gained filtered liquid carries out underpressure distillation, and pressure-controlling is at 0.2Mpa, and temperature controls at 50 DEG C.
(3) filtered liquid is through macroporous resin adsorption to saturated, and macroporous resin model is AB-8 type resin, and the aspect ratio of resin column is 8: 1-15: 1, is adsorbed as Static Adsorption or dynamic adsorption.
(4) at normal temperatures and pressures, with 1BV/h flow velocity, first use distilled water wash-out, elution volume is 3BV, washes the water-soluble impurity in the black matrimony vine aqueous solution off.
(5) with the ethanol of 70% concentration, elution volume is carry out wash-out under 8BV, uses tlc tracing detection, collects each stepwise elution liquid of the black matrimony vine aqueous solution.
(6) elutriant is at pressure-0.07 ~ 0.08Mpa, and under 60 DEG C of conditions, through decompression recycling ethanol, obtain black matrimony vine concentrated solution, its proportion is 1.08 ~ 1.12.
(7) concentrated solution carries out vacuum-drying at 70 ~ 80 DEG C, and obtain black matrimony vine anthocyanidin finished product, moisture controlled is below 5%, and content is more than 25%.
Embodiment 2: the invention provides a kind of method utilizing anthocyanidin in the black matrimony vine of acid extraction enriching and purifying, its step comprises:
(1) black matrimony vine is broken, cross 70 mesh sieves, be that the inorganic acid aqueous solution of 0.5% mixes respectively with concentration, solid-liquid ratio is 1: 8, regulates pH value 1.0, and carry out insulation and extract, the temperature that insulation is extracted, at 60 DEG C, is extracted 2.5 hours, filters.
(2) gained filtered liquid carries out underpressure distillation, and pressure-controlling is at 0.1 ~ 0.2Mpa, and temperature controls at 50 ~ 60 DEG C.
(3) filtered liquid is through macroporous resin adsorption to saturated, and macroporous resin model is DM-130 type resin, and the aspect ratio of resin column is 8: 1-15: 1, is adsorbed as Static Adsorption or dynamic adsorption.
(4) at normal temperatures and pressures, with 1BV/h flow velocity, first use distilled water wash-out, elution volume is 5BV, washes the water-soluble impurity in the black matrimony vine aqueous solution off.
(5) with the ethanol of 90% concentration, elution volume is carry out wash-out under 6BV, uses tlc tracing detection, collects each stepwise elution liquid of the black matrimony vine aqueous solution.
(6) elutriant is at pressure-0.07 ~ 0.08Mpa, and under 60 DEG C of conditions, through decompression recycling ethanol, obtain black matrimony vine concentrated solution, its proportion is 1.12.
(7) concentrated solution carries out vacuum-drying at 70 ~ 80 DEG C, and obtain black matrimony vine anthocyanidin finished product, moisture controlled is below 5%, and content is more than 25%.
Embodiment 3: the invention provides a kind of method utilizing anthocyanidin in the black matrimony vine of acid extraction enriching and purifying, its step comprises:
(1) black matrimony vine is broken, cross 80 mesh sieves, be that the inorganic acid aqueous solution of 0.7% mixes respectively with concentration, solid-liquid ratio is 1: 9, regulates pH value 2.0, and carry out insulation and extract, the temperature that insulation is extracted, at 60 DEG C, is extracted 2 hours, filters.
(2) gained filtered liquid carries out underpressure distillation, and pressure-controlling is at 0.1 ~ 0.2Mpa, and temperature controls at 60 DEG C.
(3) filtered liquid is through macroporous resin adsorption to saturated, and macroporous resin model is NKA-II type resin, and the aspect ratio of resin column is 8: 1-15: 1, is adsorbed as Static Adsorption or dynamic adsorption.
(4) at normal temperatures and pressures, with 1BV/h flow velocity, first use distilled water wash-out, elution volume is 5BV, washes the water-soluble impurity in the black matrimony vine aqueous solution off.
(5) with the ethanol of 80% concentration, elution volume is carry out wash-out under 8BV, uses tlc tracing detection, collects each stepwise elution liquid of the black matrimony vine aqueous solution.
(6) elutriant is at pressure-0.07 ~ 0.08Mpa, and under 60 DEG C of conditions, through decompression recycling ethanol, obtain black matrimony vine concentrated solution, its proportion is 1.08 ~ 1.12.
(7) concentrated solution carries out vacuum-drying at 80 DEG C, and obtain black matrimony vine anthocyanidin finished product, moisture controlled is below 5%, and content is more than 25%.
Claims (2)
1. the invention provides a kind of method utilizing anthocyanidin in the black matrimony vine of acid extraction enriching and purifying, its step comprises:
(1) black matrimony vine is broken, sieving, is that the inorganic acid aqueous solution of 0.3% ~ 0.7% mixes respectively with concentration, solid-liquid ratio is 1: 8 ~ 1: 10, regulates pH value 1.0 ~ 2.0, carries out insulation and extracts, the temperature that insulation is extracted, at 50 ~ 60 DEG C, is extracted 2 ~ 3 hours, filters.
(2) gained filtered liquid carries out underpressure distillation, and pressure-controlling is at 0.1 ~ 0.2Mpa, and temperature controls at 50 ~ 60 DEG C.
(3) filtered liquid is through macroporous resin adsorption to saturated, and macroporous resin model is the one in HPD400, DM-130, AB-8 and NKA-II type resin, and the aspect ratio of resin column is 8: 1-15: 1, is adsorbed as Static Adsorption or dynamic adsorption.
(4) at normal temperatures and pressures, with 1BV/h flow velocity, first use distilled water wash-out, elution volume is 3-5BV, washes the water-soluble impurity in the black matrimony vine aqueous solution off.
(5) with the ethanol of 70% ~ 90% concentration, elution volume is carry out wash-out under 6-8BV, uses tlc tracing detection, collects each stepwise elution liquid of the black matrimony vine aqueous solution.
(6) elutriant is at pressure-0.07 ~ 0.08Mpa, and under 50 ~ 60 DEG C of conditions, through decompression recycling ethanol, obtain black matrimony vine concentrated solution, its proportion is 1.08 ~ 1.12.
(7) concentrated solution carries out vacuum-drying at 70 ~ 80 DEG C, and obtain black matrimony vine anthocyanidin finished product, moisture controlled is below 5%, and its content is more than 25%.
2. a kind of method utilizing anthocyanidin in the black matrimony vine of acid extraction enriching and purifying according to claim 1, is characterized in that: in described step (1), and broken to cross grit number be 60-80 order.
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| CN201510761428.2A CN105384716A (en) | 2015-11-06 | 2015-11-06 | Method for enriching and purifying lycium ruthenicum Murr anthocyanin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218821A (en) * | 2018-03-29 | 2018-06-29 | 武汉雅仕博科技有限公司 | The method extracted from acorn cup, purify anthocyanidin |
| CN108440480A (en) * | 2018-04-04 | 2018-08-24 | 北京国康本草物种生物科学技术研究院有限公司 | The extracting method of lycium ruthenicum procyanidins and obtained extract |
| CN108991471A (en) * | 2018-06-27 | 2018-12-14 | 浙江农林大学暨阳学院 | A kind of natural additive for foodstuff with potent antioxidant activity |
| CN109400569A (en) * | 2018-10-18 | 2019-03-01 | 赣州华汉生物科技有限公司 | A kind of method of extraction purification anthocyanidin in butterfly Tofu pudding |
| CN111777585A (en) * | 2020-07-24 | 2020-10-16 | 哈工大机器人南昌智能制造研究院 | Preparation method of high-purity lycium ruthenicum anthocyanin powder |
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| CN104789612A (en) * | 2015-03-24 | 2015-07-22 | 乌鲁木齐益广康源生物科技有限公司 | Anthocyanin extracted from Lycium ruthenicum Murr fruit and preparation method of anthocyanin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218821A (en) * | 2018-03-29 | 2018-06-29 | 武汉雅仕博科技有限公司 | The method extracted from acorn cup, purify anthocyanidin |
| CN108440480A (en) * | 2018-04-04 | 2018-08-24 | 北京国康本草物种生物科学技术研究院有限公司 | The extracting method of lycium ruthenicum procyanidins and obtained extract |
| CN108991471A (en) * | 2018-06-27 | 2018-12-14 | 浙江农林大学暨阳学院 | A kind of natural additive for foodstuff with potent antioxidant activity |
| CN108991471B (en) * | 2018-06-27 | 2021-11-23 | 浙江农林大学暨阳学院 | Natural food additive with strong antioxidant activity |
| CN109400569A (en) * | 2018-10-18 | 2019-03-01 | 赣州华汉生物科技有限公司 | A kind of method of extraction purification anthocyanidin in butterfly Tofu pudding |
| CN111777585A (en) * | 2020-07-24 | 2020-10-16 | 哈工大机器人南昌智能制造研究院 | Preparation method of high-purity lycium ruthenicum anthocyanin powder |
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Application publication date: 20160309 |