CN102274269A - Method for extracting pigments from bracteatum leaves - Google Patents
Method for extracting pigments from bracteatum leaves Download PDFInfo
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- CN102274269A CN102274269A CN201110264827XA CN201110264827A CN102274269A CN 102274269 A CN102274269 A CN 102274269A CN 201110264827X A CN201110264827X A CN 201110264827XA CN 201110264827 A CN201110264827 A CN 201110264827A CN 102274269 A CN102274269 A CN 102274269A
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- vaccinium bracteatum
- bracteatum thunb
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Abstract
The invention relates to a method for extracting pigments from bracteatum leaves. The method comprises the following steps of: (1) crushing dried bracteatum leaves, adding 5 percent acetic acid solution in an amount which is 2 to 5 times that of the dried bracteatum leaves, soaking for 2 to 4 hours, extracting for 2 to 4 times, and filtering by using an 80 to 160-mesh filter screen to obtain filter liquor; (2) performing centrifugal separation at high speed of between 2,500 and 2,900 revolutions per minute on the filter liquor; and (3) adding supernate into a membrane separation system, performing ultrafiltration and nanofiltration to obtain concentrated solution, adding water, dispersing, adsorbing on a polyamide column, washing impurities off by using the water, eluting by using 5 to 7 resin bed volumes (BV) of 50 percent ethanol solution, concentrating eluent, freezing and drying to obtain the pigments from the bracteatum leaves. The pigments extracted from the bracteatum leaves is high in stability and purity, less in energy consumption in the production process and small in pollution, and is suitable for industrial production.
Description
Technical field
The invention belongs to biological technical field, especially relate to a kind of method of extracting pigment in the leaf of Vaccinium bracteatum Thunb..
Background technology
Fructus Vaccinii Bracteati (
Vaccinium bracteatumThunb
.) be Ericaceae Vaccinium plant, have another name called Vaccinium bracteatum Thunb., Fructus Vaccinii Fragilis etc.Effective ingredient has cyanine glycoside, flavonoid, tannin class, triterpenes etc. in the Fructus Vaccinii Bracteati branch and leaf, the black-and-blue cellulose content height of water solublity wherein has and promotes it is erythropsin resynthesis, Vp model machine energy, improves blood microcirculation, antiulcer, anti-inflammatory, the anti-ageing multiple physiologically active of waiting for a long time.
Bibliographical information (Hu Zhijie etc. are arranged, leaf of Vaccinium bracteatum Thunb. pigment extraction process and pigment character are studied [J] again. Chinese wild plant resource, 2001,22(4): 47-48) leaf of Vaccinium bracteatum Thunb. pigment extractum color body darkly has Arillus Longan fragrance, free from extraneous odour, has stronger hygroscopicity, soluble in water, be slightly soluble in 75% ethanol, be insoluble to ether and oils.Pigment light resistance, reducing resistance are strong, oxidative resistance a little less than, more stable under acid condition.
Water or organic solvent method are adopted in the extraction of present domestic leaf of Vaccinium bracteatum Thunb. pigment more, also utilize the supercritical carbon dioxide extraction method that leaf of Vaccinium bracteatum Thunb. is studied, but the cost of supercritical carbon dioxide extraction method and equipment requirements height, feasibility is restricted.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting pigment in the leaf of Vaccinium bracteatum Thunb..
The objective of the invention is to be achieved through the following technical solutions:
(1) exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, added 12-18 and doubly measure 5% acetum immersion 2-4 hour, extract 2-3 time, filter, obtain filtrate with 80-160 purpose filter screen;
(2) filtrate is carried out the high speed centrifugation separation of 2500-2900rpm, obtains supernatant;
(3) supernatant adds ultrafiltration in the film separation system, nanofiltration, obtains concentrated solution;
(4) concentrated solution adds aqueous dispersion, and last polyamide column absorption washes decontamination earlier with water, reuse 5-7BV50% alcoholic solution eluting, and eluent concentrates, and lyophilization promptly gets the leaf of Vaccinium bracteatum Thunb. pigment.
Ultrafilter membrane is that molecular cut off is the ultrafilter membrane of 3000-10000 in the described step (3).
NF membrane is that molecular cut off is the NF membrane of 200-300 in the described step (3).
Technical advantage of the present invention is: the present invention's acetum lixiviate can increase the stripping of pigment; Adopt membrane filtration to belong to the physics remove impurity, not only energy consumption is low, pollution is little, can also reduce the Yin Gaowen pigment and decompose, and improves yield.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to the following example.
The specific embodiment
Embodiment 1:
Exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, take by weighing 500g, adding 12 times of amount 5% acetums soaked 4 hours, extract 3 times, filter, obtain filtrate with 80 purpose filter screens, the high speed centrifugation that carries out 2900rpm separates, supernatant adds ultrafiltration in the film separation system, and the ultrafilter membrane molecular cut off is 3000-10000, nanofiltration, the NF membrane molecular cut off is 200-300, obtain concentrated solution, add aqueous dispersion, last polyamide column absorption, wash decontamination earlier with water, reuse 7BV50% alcoholic solution eluting, eluent concentrates, and lyophilization promptly gets leaf of Vaccinium bracteatum Thunb. pigment 23g.
Embodiment 2:
Exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, take by weighing 1kg, add 18 times of amount 5% acetums and soak extraction in 3 hours 3 times, filter with 160 purpose filter screens, obtain filtrate, the high speed centrifugation that carries out 2500rpm separates, and supernatant adds ultrafiltration in the film separation system, the ultrafilter membrane molecular cut off is 3000-10000, nanofiltration, the NF membrane molecular cut off is 200-300, obtains concentrated solution, add aqueous dispersion, last polyamide column absorption washes decontamination earlier with water, reuse 5BV50% alcoholic solution eluting, eluent concentrates, and lyophilization promptly gets leaf of Vaccinium bracteatum Thunb. pigment 56g.
Embodiment 3:
Exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, take by weighing 1kg, add 15 times of amount 5% acetums and soak extraction in 2 hours 2 times, filter with 160 purpose filter screens, obtain filtrate, the high speed centrifugation that carries out 2500rpm separates, and supernatant adds ultrafiltration in the film separation system, the ultrafilter membrane molecular cut off is 3000-10000, nanofiltration, the NF membrane molecular cut off is 200-300, obtains concentrated solution, add aqueous dispersion, last polyamide column absorption washes decontamination earlier with water, reuse 6BV50% alcoholic solution eluting, eluent concentrates, and lyophilization promptly gets leaf of Vaccinium bracteatum Thunb. pigment 68g.
Embodiment 3:
Exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, take by weighing 5kg, add 16 times of amount 5% acetums and soak extraction in 3 hours 3 times, filter with 100 purpose filter screens, obtain filtrate, the high speed centrifugation that carries out 2900rpm separates, and supernatant adds ultrafiltration in the film separation system, the ultrafilter membrane molecular cut off is 3000-10000, nanofiltration, the NF membrane molecular cut off is 200-300, obtains concentrated solution, add aqueous dispersion, last polyamide column absorption washes decontamination earlier with water, reuse 7BV50% alcoholic solution eluting, eluent concentrates, and lyophilization promptly gets leaf of Vaccinium bracteatum Thunb. pigment 333g.
Embodiment 3:
Exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, take by weighing 5kg, add 12 times of amount 5% acetums and soak extraction in 2 hours 2 times, filter with 160 purpose filter screens, obtain filtrate, the high speed centrifugation that carries out 2800rpm separates, and supernatant adds ultrafiltration in the film separation system, the ultrafilter membrane molecular cut off is 3000-10000, nanofiltration, the NF membrane molecular cut off is 200-300, obtains concentrated solution, add aqueous dispersion, last polyamide column absorption washes decontamination earlier with water, reuse 7BV50% alcoholic solution eluting, eluent concentrates, and lyophilization promptly gets leaf of Vaccinium bracteatum Thunb. pigment 356g.
Embodiment 3:
Exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, take by weighing 10kg, add 18 times of amount 5% acetums and soak extraction in 2 hours 3 times, filter with 160 purpose filter screens, obtain filtrate, the high speed centrifugation that carries out 2900rpm separates, and supernatant adds ultrafiltration in the film separation system, the ultrafilter membrane molecular cut off is 3000-10000, nanofiltration, the NF membrane molecular cut off is 200-300, obtains concentrated solution, add aqueous dispersion, last polyamide column absorption washes decontamination earlier with water, reuse 6BV50% alcoholic solution eluting, eluent concentrates, and lyophilization promptly gets leaf of Vaccinium bracteatum Thunb. pigment 652g.
Claims (3)
1. method of extracting pigment in the leaf of Vaccinium bracteatum Thunb. is characterized in that:
(1) exsiccant leaf of Vaccinium bracteatum Thunb. is pulverized, added 12-18 and doubly measure 5% acetum immersion 2-4 hour, extract 2-3 time, filter, obtain filtrate with 80-160 purpose filter screen;
(2) filtrate is carried out the high speed centrifugation separation of 2500-2900rpm, obtains supernatant;
(3) supernatant adds ultrafiltration in the film separation system, nanofiltration, obtains concentrated solution;
(4) concentrated solution adds aqueous dispersion, and last polyamide column absorption washes decontamination earlier with water, reuse 5-7BV50% alcoholic solution eluting, and eluent concentrates, and lyophilization promptly gets the leaf of Vaccinium bracteatum Thunb. pigment.
2. a kind of according to claim 1 method of extracting pigment in the leaf of Vaccinium bracteatum Thunb. is characterized in that ultrafilter membrane is that molecular cut off is the ultrafilter membrane of 3000-10000 in the described step (3).
3. a kind of according to claim 1 method of extracting pigment in the leaf of Vaccinium bracteatum Thunb. is characterized in that NF membrane is that molecular cut off is the NF membrane of 200-300 in the described step (3).
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103113756A (en) * | 2013-03-06 | 2013-05-22 | 无锡市金和泰农业生物技术有限公司 | Method for efficiently extracting and preparing vaccinium leaves pigment |
CN103408964A (en) * | 2013-08-15 | 2013-11-27 | 宜兴市红豆杉生态科技有限公司 | Method for improving extraction yield of melanin in Vaccinium bracteatum Thunb by using polyphenol oxidase and tea polyphenol |
CN108354111A (en) * | 2018-01-08 | 2018-08-03 | 浙江大学 | Natural colorant and its preparation method and application based on oriental blueberry leaf |
CN109097413A (en) * | 2018-08-01 | 2018-12-28 | 江南大学 | A method of the different indigo pigments of tone are prepared based on Vaccinium bracteatum Thunb. Leaves |
CN117024988A (en) * | 2023-07-24 | 2023-11-10 | 浙江旺林生物科技有限公司 | Method for extracting Vaccinium bracteatum leaf melanin |
-
2011
- 2011-09-08 CN CN201110264827XA patent/CN102274269A/en active Pending
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103113756A (en) * | 2013-03-06 | 2013-05-22 | 无锡市金和泰农业生物技术有限公司 | Method for efficiently extracting and preparing vaccinium leaves pigment |
CN103113756B (en) * | 2013-03-06 | 2014-12-10 | 无锡市金和泰农业生物技术有限公司 | Method for efficiently extracting and preparing vaccinium leaves pigment |
CN103408964A (en) * | 2013-08-15 | 2013-11-27 | 宜兴市红豆杉生态科技有限公司 | Method for improving extraction yield of melanin in Vaccinium bracteatum Thunb by using polyphenol oxidase and tea polyphenol |
CN103408964B (en) * | 2013-08-15 | 2014-12-10 | 宜兴市红豆杉生态科技有限公司 | Method for improving extraction yield of melanin in Vaccinium bracteatum Thunb by using polyphenol oxidase and tea polyphenol |
CN108354111A (en) * | 2018-01-08 | 2018-08-03 | 浙江大学 | Natural colorant and its preparation method and application based on oriental blueberry leaf |
CN108354111B (en) * | 2018-01-08 | 2022-05-17 | 浙江大学 | Natural colorant based on Vaccinium bracteatum leaves, and preparation method and application thereof |
CN109097413A (en) * | 2018-08-01 | 2018-12-28 | 江南大学 | A method of the different indigo pigments of tone are prepared based on Vaccinium bracteatum Thunb. Leaves |
CN109097413B (en) * | 2018-08-01 | 2020-12-29 | 江南大学 | Method for preparing indigo pigment with different colors based on vaccinium bracteatum leaves |
CN117024988A (en) * | 2023-07-24 | 2023-11-10 | 浙江旺林生物科技有限公司 | Method for extracting Vaccinium bracteatum leaf melanin |
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