CN104945365A - Technology for extracting anthocyanidin from black rice - Google Patents

Technology for extracting anthocyanidin from black rice Download PDF

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Publication number
CN104945365A
CN104945365A CN201510297289.2A CN201510297289A CN104945365A CN 104945365 A CN104945365 A CN 104945365A CN 201510297289 A CN201510297289 A CN 201510297289A CN 104945365 A CN104945365 A CN 104945365A
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Prior art keywords
black rice
powder
anthocyanidin
technique
extraction
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CN201510297289.2A
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陈玲华
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陈玲华
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic 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
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulfur atoms in positions 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulfur atoms in positions 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulfur atoms in positions 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins

Abstract

The invention discloses a technology for extracting anthocyanidin from black rice and relates to the field of a plant extraction technology. The method comprises the following steps: (1) pretreatment: crushing black rice into a powder with its fineness of 60-80 meshes; (2) extraction: mixing black rice powder and water, adjusting pH value of the mixed liquid to 4-6, and immersing under the condition of water bath at 50 DEG C for 1-2h; and centrifuging with a high speed centrifuge and taking a supernatant for later use; (3) ultrafiltration extraction: filtering by putting the supernatant obtained from the step (2) into a feed liquid barrel of 3000Da ultrafiltration membrane equipment and collecting an effluent for later use; (4) purification: adsorbing the effluent obtained from the step (3) through macroporous resin; eluting with ethanol after adsorption, and collecting an eluate; and prefreezing the eluate and finally freeze-drying by putting the prefrozen eluate into a vacuum freeze drier so as to obtain a claret-colored black rice anthocyanins powder. The method provided by the invention has advantages of simple operation and extraction efficiency.

Description

A kind of technique extracting anthocyanidin from black rice
Technical field
The present invention relates to technical field of plant extraction, especially relate to a kind of technique extracting anthocyanidin from black rice.
Background technology
Anthocyanidin (Anthocyanidin), also known as cyanidin(e), is the water-soluble natural pigment that nature one class is extensively present in plant, and belonging to flavonoids, is also the main color-generation material in plant petals.Anthocyanidin is the antidotal nutritious supplementary of pure natural, research proves mankind nowadays and finds most good antioxidant, its antioxidant property exceeds 50 times than vitamin-E, 20 times are exceeded than vitamins C, it is 100% to the biological effectiveness of human body, within 20 minutes, just can detect in blood after taking, and active 75 hours can be preserved in blood of human body.Anthocyanidin can protect human body from objectionable impurities---and the damage of free radical, contributes to preventing the multiple disease relevant with free radical.Anthocyanidin can also strengthen blood vessel elasticity, and protection arteries inwall, reduces blood pressure.Anthocyanidin can promote the slickness of skin, U.S. face skin, and all right inflammation-inhibiting and allergy, improve the snappiness in joint, prevention sacroiliitis.Except this, anthocyanidin can also promote that the rhodopsin in retina cell regenerates, and improves eyesight, also has radiation-resistant effect.
Black rice is commonly called as " medicine rice ", " long-lived rice ", " angle's rice ", " rice of enriching blood ".Ancient agriculture medical book is recorded: black rice " improving eyesight is invigorated blood circulation for enriching yin and nourishing kidney, body-building warming stomach, clearing liver ease constipation, sliding wet benefit essence, and tonifying lung delays muscle ".Black rice has very high nutritive value and pharmaceutical use, it is not only containing the necessary amino acid of human body, unsaturated fatty acids, rich in protein, VB1, VB2 and VC, also be rich in the mineral nutrient elements such as iron, zinc, copper, calcium, the composition that anthocyanidin, carotene and the chlorophyll etc. that more lack containing rice are special.The processing of current domestic black rice focuses on the exploitation of black-rice health-care food, such as: make black rice bread, black rice eight treasure gruel, black rice nourishing sesame cream, black rice bifid Yoghourt and five black nutritive mediums etc., still rest on the preliminary working stage to the comprehensive utilization of black rice, it is lower that product transforms earned value techniques level.Therefore, utilize black rice to extract anthocyanidin as natural additive, the added value of black rice can be improved, there is important economic benefit and social benefit.
Summary of the invention
Goal of the invention of the present invention is: for above-mentioned Problems existing, there is provided a kind of technique extracting anthocyanidin from black rice, method of the present invention has easy and simple to handle, extraction efficiency advantages of higher, a kind of new approach can be provided for the utilization of black rice, improve the added value of black rice.
To achieve these goals, the technical solution used in the present invention is as follows:
From black rice, extract a technique for anthocyanidin, this technique comprises the following steps:
(1) pre-treatment: black rice flour being broken to fineness is 60-80 object powder, obtains black rice powder;
(2) extract: be that the ratio of 1:5-15 mixes with mass ratio by black rice flour and water, then after the pH value of mixed solution being adjusted to 4-6 with hydrochloric acid, be soak 1-2h under the water bath condition of 50 DEG C in temperature; Then use supercentrifuge centrifugal 15min under the speed of 4000rpm, get supernatant liquor for subsequent use;
(3) ultrafiltration extraction: feed liquid bucket step (2) gained supernatant liquor being put into the device for ultrafiltration membrane of 3000Da, red-tape operati pressure is 0.3Mpa, adopts the water-cooled mode of flowing, under keeping solution to be in room temperature, time is 8-12h, collects effluent liquid for subsequent use;
(4) purifying: the effluent liquid of step (3) gained is adsorbed by macroporous resin; Adsorb rear ethanol elution, collect elutriant; Put into vacuum freeze drier lyophilize after elutriant is carried out precooling to moisture content below 5%, control vacuum tightness at below 15Pa, temperature is less than-40 DEG C, obtains mauve black rice anthocyanin powder after drying completely.
Further, in described step (2), the weight ratio of extraction agent and black rice powder is 1:10.
Further, described macroporous resin is the one in AB-8, DM130 or ADS-17.
Further, when adsorbing with macroporous resin, coutroi velocity is 1.0-1.5mL/min.
Further, concentration is adopted in described step (4) to be that the ethanol of 60%-80%v/v carries out wash-out.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows:
1, the present invention extracts anthocyanidin from black rice, by regulating and controlling optimum solid-liquid ratio, extraction time, Extracting temperature, filtration condition, the factors such as purifying process, shortening extraction time, increasing the extraction yield of effective constituent.The condition extracted both ensure that the low-temperature short-time of effective ingredient extracted, and in turn ensure that the time.There is technique simple, easy handling, extraction yield advantages of higher.
2, the macroporous resin selected in purge process of the present invention all has good adsorption effect, effectively removes the impurity such as vegetable polysaccharides, albumen, and the DNA purity of anthocyanidin is high, simplifies extraction process.Adopt the ethanol of 50%-60% as eluent, it is convenient to reclaim, environmentally safe.
3, the present invention strengthens the comprehensive utilization of black rice, improves the added value of black rice, for increasing peasant income provide a kind of new approach.
Embodiment
The invention discloses a kind of technique extracting anthocyanidin from black rice, undertaken testing and improving by the aspect such as control, the adjustment of Extracting temperature, the optimization of purifying process from solid-liquid ratio, reach the object improving black rice anthocyanin extraction yield.Below by way of specific embodiment, the invention will be further described.
Embodiment 1
From black rice, extract a technique for anthocyanidin, this technique comprises the following steps successively:
(1) pre-treatment: take 500g black rice, being crushed to fineness is 60 object powder, obtains black rice powder;
(2) extract: be that the ratio of 1:5 mixes with mass ratio by black rice flour and water, then after the pH value of mixed solution being adjusted to 4 with hydrochloric acid, be soak 2h under the water bath condition of 50 DEG C in temperature; Then use supercentrifuge centrifugal 15min under the speed of 4000rpm, get supernatant liquor for subsequent use;
(3) ultrafiltration extraction: feed liquid bucket step (2) gained supernatant liquor being put into the device for ultrafiltration membrane of 3000Da, red-tape operati pressure is 0.3Mpa, adopts the water-cooled mode of flowing, under keeping solution to be in room temperature, time is 8h, collects effluent liquid for subsequent use;
(4) purifying: the effluent liquid of step (3) gained is adsorbed by macroporous resin AB-8, coutroi velocity is 1.0mL/min; Having adsorbed rear employing concentration is that the ethanol of 80%v/v carries out wash-out, collects elutriant; Put into vacuum freeze drier lyophilize after elutriant is carried out precooling to moisture content below 5%, control vacuum tightness at below 15Pa, temperature is less than-40 DEG C, obtains mauve black rice anthocyanin powder after drying completely.
Through calculating, the present embodiment last gained anthocyanidin powder total amount is 5.8g.
Embodiment 2
From black rice, extract a technique for anthocyanidin, this technique comprises the following steps successively:
(1) pre-treatment: take 500g black rice, being crushed to fineness is 80 object powder, obtains black rice powder;
(2) extract: be that the ratio of 1:12 mixes with mass ratio by black rice flour and water, then after the pH value of mixed solution being adjusted to 4 with hydrochloric acid, be soak 1h under the water bath condition of 50 DEG C in temperature; Then use supercentrifuge centrifugal 15min under the speed of 4000rpm, get supernatant liquor for subsequent use;
(3) ultrafiltration extraction: feed liquid bucket step (2) gained supernatant liquor being put into the device for ultrafiltration membrane of 3000Da, red-tape operati pressure is 0.3Mpa, adopts the water-cooled mode of flowing, under keeping solution to be in room temperature, time is 8-12h, collects effluent liquid for subsequent use;
(4) purifying: the effluent liquid of step (3) gained is adsorbed by macroporous resin DM130, coutroi velocity is 1.5mL/min; Having adsorbed rear employing concentration is that the ethanol of 60%v/v carries out wash-out, collects elutriant; Put into vacuum freeze drier lyophilize after elutriant is carried out precooling to moisture content below 5%, control vacuum tightness at below 15Pa, temperature is less than-40 DEG C, obtains mauve black rice anthocyanin powder after drying completely.
Through calculating, the present embodiment last gained anthocyanidin powder total amount is 5.9g.
Embodiment 3
From black rice, extract a technique for anthocyanidin, this technique comprises the following steps successively:
(1) pre-treatment: take 500g black rice, being crushed to fineness is 80 object powder, obtains black rice powder;
(2) extract: be that the ratio of 1:10 mixes with mass ratio by black rice flour and water, then after the pH value of mixed solution being adjusted to 4 with hydrochloric acid, be soak 2h under the water bath condition of 50 DEG C in temperature; Then use supercentrifuge centrifugal 15min under the speed of 4000rpm, get supernatant liquor for subsequent use;
(3) ultrafiltration extraction: feed liquid bucket step (2) gained supernatant liquor being put into the device for ultrafiltration membrane of 3000Da, red-tape operati pressure is 0.3Mpa, adopts the water-cooled mode of flowing, under keeping solution to be in room temperature, time is 12h, collects effluent liquid for subsequent use;
(4) purifying: the effluent liquid of step (3) gained is adsorbed by macroporous resin AB-8, coutroi velocity is 1.2mL/min; Having adsorbed rear employing concentration is that the ethanol of 80%v/v carries out wash-out, collects elutriant; Put into vacuum freeze drier lyophilize after elutriant is carried out precooling to moisture content below 5%, control vacuum tightness at below 15Pa, temperature is less than-40 DEG C, obtains mauve black rice anthocyanin powder after drying completely.
Through calculating, the present embodiment last gained anthocyanidin powder total amount is 6.1g.
Embodiment 4
From black rice, extract a technique for anthocyanidin, this technique comprises the following steps successively:
(1) pre-treatment: take 500g black rice, being crushed to fineness is 60 object powder, obtains black rice powder;
(2) extract: be that the ratio of 1:15 mixes with mass ratio by black rice flour and water, then after the pH value of mixed solution being adjusted to 6 with hydrochloric acid, be soak 2h under the water bath condition of 50 DEG C in temperature; Then use supercentrifuge centrifugal 15min under the speed of 4000rpm, get supernatant liquor for subsequent use;
(3) ultrafiltration extraction: feed liquid bucket step (2) gained supernatant liquor being put into the device for ultrafiltration membrane of 3000Da, red-tape operati pressure is 0.3Mpa, adopts the water-cooled mode of flowing, under keeping solution to be in room temperature, time is 10h, collects effluent liquid for subsequent use;
(4) purifying: the effluent liquid of step (3) gained is adsorbed by macroporous resin AB-8, coutroi velocity is 1.5mL/min; Having adsorbed rear employing concentration is that the ethanol of 75%v/v carries out wash-out, collects elutriant; Put into vacuum freeze drier lyophilize after elutriant is carried out precooling to moisture content below 5%, control vacuum tightness at below 15Pa, temperature is less than-40 DEG C, obtains mauve black rice anthocyanin powder after drying completely.
Through calculating, the present embodiment last gained anthocyanidin powder total amount is 5.7g.
Black rice anthocyanin extraction process provided by the present invention is simple, cost is low, extraction yield is high, shows that the anthocyanidin content of this finished product is high, and has higher biological activity, have very high using value through efficient liquid phase chromatographic analysis.

Claims (5)

1. from black rice, extract a technique for anthocyanidin, it is characterized in that this technique comprises the following steps:
(1) pre-treatment: black rice flour being broken to fineness is 60-80 object powder, obtains black rice powder;
(2) extract: be that the ratio of 1:5-15 mixes with mass ratio by black rice flour and water, then after the pH value of mixed solution being adjusted to 4-6 with hydrochloric acid, be soak 1-2h under the water bath condition of 50 DEG C in temperature; Then use supercentrifuge centrifugal 15min under the speed of 4000rpm, get supernatant liquor for subsequent use;
(3) ultrafiltration extraction: feed liquid bucket step (2) gained supernatant liquor being put into the device for ultrafiltration membrane of 3000Da, red-tape operati pressure is 0.3Mpa, adopts the water-cooled mode of flowing, under keeping solution to be in room temperature, time is 8-12h, collects effluent liquid for subsequent use;
(4) purifying: the effluent liquid of step (3) gained is adsorbed by macroporous resin; Adsorb rear ethanol elution, collect elutriant; Put into vacuum freeze drier lyophilize after elutriant is carried out precooling to moisture content below 5%, control vacuum tightness at below 15Pa, temperature is less than-40 DEG C, obtains mauve black rice anthocyanin powder after drying completely.
2. a kind of technique extracting anthocyanidin from black rice according to claim 1, is characterized in that: in described step (2), the weight ratio of extraction agent and black rice powder is 1:10.
3. a kind of technique extracting anthocyanidin from black rice according to claim 1 and 2, is characterized in that: described macroporous resin is the one in AB-8, DM130 or ADS-17.
4. a kind of technique extracting anthocyanidin from black rice according to claim 3, is characterized in that: when adsorbing with punching resin, and coutroi velocity is 1.0-1.5mL/min.
5. a kind of technique extracting anthocyanidin from black rice according to claim 4, is characterized in that: adopt concentration to be the ethanol elution of 60%-80%v/v in step (4).
CN201510297289.2A 2015-06-03 2015-06-03 Technology for extracting anthocyanidin from black rice Pending CN104945365A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105777699A (en) * 2016-05-19 2016-07-20 湖北紫鑫生物科技有限公司 Preparation method of black rice anthocyanin without pesticide residue
CN106008626A (en) * 2016-05-27 2016-10-12 合肥工业大学 Method for rapidly preparing anthocyanin and cyanidin-3-glucoside from black rice
CN107235951A (en) * 2017-07-03 2017-10-10 中南林业科技大学 A kind of new method of the high efficiency extraction anthocyanidin from black rice
CN109170886A (en) * 2018-09-12 2019-01-11 陈晨 A method of the extraction anthocyanidin content from purple rice shell can be improved
CN110437197A (en) * 2019-07-31 2019-11-12 湖南华诚生物资源股份有限公司 A method of extracting anthocyanidin from butterfly Tofu pudding

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102766125A (en) * 2011-08-04 2012-11-07 张文佳 Extraction and purification method for black rice anthocyanin

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Publication number Priority date Publication date Assignee Title
CN102766125A (en) * 2011-08-04 2012-11-07 张文佳 Extraction and purification method for black rice anthocyanin

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张文佳等: "黑米花青素提取与纯化工艺研究", 《安徽农业科学》 *
薛晓丽: "HPLC法测定黑米中花青素的主要成分及含量", 《安徽农业科学》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105777699A (en) * 2016-05-19 2016-07-20 湖北紫鑫生物科技有限公司 Preparation method of black rice anthocyanin without pesticide residue
CN106008626A (en) * 2016-05-27 2016-10-12 合肥工业大学 Method for rapidly preparing anthocyanin and cyanidin-3-glucoside from black rice
CN106008626B (en) * 2016-05-27 2018-07-13 合肥工业大学 A kind of method of quick preparation black rice anthocyanin Cy-3-G
CN107235951A (en) * 2017-07-03 2017-10-10 中南林业科技大学 A kind of new method of the high efficiency extraction anthocyanidin from black rice
CN109170886A (en) * 2018-09-12 2019-01-11 陈晨 A method of the extraction anthocyanidin content from purple rice shell can be improved
CN110437197A (en) * 2019-07-31 2019-11-12 湖南华诚生物资源股份有限公司 A method of extracting anthocyanidin from butterfly Tofu pudding
CN110437197B (en) * 2019-07-31 2021-04-13 湖南华诚生物资源股份有限公司 Method for extracting anthocyanin from sphenoidea

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Application publication date: 20150930