CN103113756B - Method for efficiently extracting and preparing vaccinium leaves pigment - Google Patents
Method for efficiently extracting and preparing vaccinium leaves pigment Download PDFInfo
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- CN103113756B CN103113756B CN201310070246.1A CN201310070246A CN103113756B CN 103113756 B CN103113756 B CN 103113756B CN 201310070246 A CN201310070246 A CN 201310070246A CN 103113756 B CN103113756 B CN 103113756B
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Abstract
The invention discloses a method for efficiently extracting and preparing vaccinium leaves pigment. The method comprises the following steps of: cleaning vaccinium leaves with water, mechanically crushing, extracting through an ultrasound-microwave assistive technology by using water as an extraction solvent, refrigerating and centrifuging an extracting solution to remove precipitation, taking supernatant liquid, carrying out microfiltration and purification on a ceramic membrane and concentrating the supernatant liquid, carrying out freeze drying on a concentrated solution to prepare the vaccinium leaves pigment. The method can greatly improve the yield and purity of the vaccinium leaves pigment, the extracted and prepared vaccinium leaves pigment is good in safety, strong in biological activity, simple in extraction technology, short in time, little in energy consumption, low in cost and high in efficiency, and the method is complete green production, so that the method is suitable for industrial production.
Description
Technical field
The present invention relates to agricultural-food, food processing technology field, especially relate to a kind of method that high efficiency extraction is prepared myrtillin leave pigment.
Background technology
Fructus Vaccinii Bracteati plant belongs to Ericaceae, has long applicating history in China, no matter is as food, or as medicine, is all very distinctive.The research of Vaccinium bracteatum Thunb. Leaves is almost to blank abroad, the domestic research report that has had pair Vaccinium bracteatum Thunb. Leaves pigment extraction aspect.The people such as Wang Li utilize polygalacturonase and cellulase, and under buffer conditions, to Vaccinium bracteatum Thunb. Leaves, melanic extraction is studied, and discovery polygalacturonase and cellulase share and be conducive to improve melanic yield.The people such as that He'nan University of Technology is permitted is of heap of stone, the Wang Li of Southern Yangtze University, the Hu Zhijie of Nanjing Forestry University and Jiang Ping adopt ethanol as extracting solvent, and the Extraction of Pigment of myrtillin leave is studied, and have determined the optimum extraction process of pigment.China of Wei state of He'nan University of Technology adopts and uses aqueous ethanolic solution as extracting solvent, adopts the ultrasonic frequency of 59KHz to extract myrtillin leave pigment, has determined the optimum extraction process of pigment.That Agricultural University Of Nanjing Du builds is bright, Jiangsu Province's hormone institute history is built the people such as intelligent using water as extracting solvent, then adds alum at 50-60 DEG C, myrtillin leave pigment to be extracted.The people such as Yu Qing adopt traditional solvent and Mierocrystalline cellulose enzyme process to extract myrtillin leave pigment, have determined the optimised process of solvent-extraction process.The patent " a kind of method of extracting pigments from bracteatum leaves " (application number: 201110264827.X) of Nanjing Zelang Pharmaceutical Technology Inc.'s application, dry myrtillin leave is pulverized in this invention, add acetum to soak, then extract, obtain filtrate by filter screen, filtrate high speed centrifugation separates, obtain supernatant liquor, supernatant liquor adds ultrafiltration in film separating system, nanofiltration, obtain concentrated solution, after polyamide column absorption, use ethanolic soln wash-out, elutriant is concentrated, and lyophilize obtains myrtillin leave pigment.Patent that University Of Agriculture and Forestry In Fujian the declares method of extraction of natural melanin " a kind of from myrtillin leave " (patent No.: ZL200510104210.6), this invention adopts zymin in conjunction with solvent extraction natural black pigment.The patent " the melanic manufacture method of a kind of water miscible plant " (application number: 201110097948.X) of Zhejiang Medicine Co's application, melanin precursor is manufactured in this invention taking myrtillin leave as raw material, then manufactures plant melanochrome through operations such as enzymatic oxidation, macroporous resin purification and spraying are dried.
From the research report that myrtillin leave melanochrome is extracted and the patent of declaring, be mainly to adopt following several method: (1) ethanol, as extracting solvent, adopts enzyme process assisted extraction; (2) single ethanol is as extracting solvent extraction; (3) ethanol is as extracting solvent, in conjunction with ultrasonic assisted extraction; (4), using water as extracting solvent, add alum to extract; (5) acetic acid extraction, membrane separation concentration, polyamide column absorption, myrtillin leave pigment is prepared in lyophilize; (6) Enzymatic Extraction, macroporous resin purification and spraying are dry etc., and operation is prepared myrtillin leave melanochrome.From above analysis, myrtillin leave pigment adopts organic solvent more as extracting solvent relatively at present, auxiliary extraction technology is in the majority with Enzymatic Extraction, has that solvent load is large, cost is high, the shortcoming such as, chemical agent residue unfriendly to environment, complex process in suitability for industrialized production.
Ultrasonic wave and using microwave-assisted are current emerging extracting method, microwave has selectivity, can optionally extract polar molecule, target components is directly separated, thereby the purity of product is improved, and quality is improved, and can greatly shorten extraction time simultaneously, improve extraction rate, pollution-free, effective component yield is high.Ultrasonic wave is to utilize ultrasonic vibrational energy can change material weave construction, state, function, has advantages of that energy consumption is low, easy and simple to handle, speed is fast, extraction yield is high, does not destroy effective ingredient.
Purge process from pigment extracts, adopts macroporous resin to carry out purifying to pigment at present mostly, and this method exists following problem: the security of (1) resin, mainly refers to the safety issue that pore-creating agent and degradation product bring; (2) adsorptive power reduces when Reusability; (3) in resin use procedure, particle may be broken; (4) be subject to the pollution of other materials and reduce separating power.
Summary of the invention
The problems referred to above that exist for prior art, a kind of method that the applicant provides myrtillin leave pigment high efficiency extraction to prepare.Present method can improve myrtillin leave pigment yield and purity greatly, extract preparation the security of myrtillin leave pigment good, biological activity is strong, extraction process is simple, the time is short, less energy consumption, cost is low, efficiency is high, and green production, is suitable for suitability for industrialized production completely.
Technical scheme of the present invention is as follows:
A method prepared by myrtillin leave pigment high efficiency extraction, comprises the following steps:
(A) pulverize: after myrtillin leave is cleaned, carry out mechanical disintegration;
(B) extract: in the myrtillin leave slag after pulverizing, add water, then carry out ultrasonic-microwave-assisted and extract;
(C) centrifugal: to adopt frozen centrifugation, remove precipitation, get supernatant liquor;
(D) purifying, concentrated: under ceramic membrane and working pressure, supernatant liquor is carried out to purifying, concentrated;
(E) preparation: concentrated solution is prepared to myrtillin leave pigment by lyophilize.
In step (B), water is as extracting solvent, and the ratio of myrtillin leave slag and water is 1:30-1:10, and unit is g/mL.The processing parameter that ultrasonic in step (B)-microwave-assisted extracts myrtillin leave pigment is: ultrasonic frequency is 40KHz, extracts temperature 40-60 DEG C, microwave power 75-95W, extraction time 20-40min.In step (C), the processing parameter of frozen centrifugation is: centrifugal rotational speed is 7000-10000rpm, and centrifugation time is 20-40min.Described in step (D), ceramic membrane aperture is 150-200nm, and working pressure is 0.095-0.130Mpa.
The technique effect that the present invention is useful is:
The present invention combines ultrasonic and microwave technology, adopt water as extracting solvent, myrtillin leave pigment is extracted, make full use of the cavatition of ultrasonic vibration and the high energy effect of microwave, improve myrtillin leave pigment yield and purity, shorten extraction time, greatly reduce production costs, simultaneously there is not chemical agent residue, solved that the solvent load that current myrtillin leave method for extracting pigment exists is large, cost is high,, chemical agent residue unfriendly to environment, extraction time are long, the technological difficulties of complex process.
The present invention adopts membrane separation technique to carry out purifying, this purification process possesses following advantage: (1) sepn process is physical sepn, separated component does not have the variation of calorifics, seldom has chemical and biological variation, can keep preferably stability and the physiologically active of pigment; (2) while concentrating, without heat of phase transformation, energy consumption is low; (3) do not consume chemical, there is no environmental pollution; (4) easy to operate, be easy to suitability for industrialized production.
The present invention adopts the method for microfiltration of ceramic membrane to carry out purifying, concentrated to myrtillin leave pigment, well keep the stable and physiologically active of pigment, do not consume chemical reagent simultaneously, can not cause environmental pollution, the structure deteriorate that does not exist the wash-out chemical reagent existing in resin adsorption method purifying pigment process may cause pigment composition, and then affect the shortcoming of the physiologically active of pigment, and adopt cryodesiccated method to prepare myrtillin leave pigment, farthest keep the physiologically active of pigment.
The complete green production of extraction preparation method of myrtillin leave pigment provided by the invention, the physiologically active of product is farthest retained, and fills up the research blank that also there is no ultrasonic-microwave-assisted high efficiency extraction myrtillin leave pigment both at home and abroad.
Embodiment
Below in conjunction with embodiment, the invention will be further described; but not as a limitation of the invention; the content that protection scope of the present invention is recorded with claim is as the criterion, and any equivalence techniques means of making according to the present invention are replaced and all do not departed from protection scope of the present invention.
Embodiment 1
A method prepared by myrtillin leave pigment high efficiency extraction, it comprises the following steps:
(A) pulverize: taking Yixing, fresh myrtillin leave is raw material, water cleans, and then passes through mechanical disintegration, stand-by;
(B) extract: according to solid-liquid ratio 1:10(g/mL) to pulverize after myrtillin leave slag in add water, set ultrasonic-microwave-assisted and extract parameter: ultrasonic frequency is 40KHz, extract 40 DEG C of temperature, microwave power 95W, extraction time 20min carries out ultrasonic-microwave-assisted and extracts under this parameter;
(C) centrifugal: to be 10000rpm at centrifugal rotational speed, under the condition of centrifugation time 20min, to carry out frozen centrifugation, remove precipitation, get supernatant liquor stand-by;
(D) purifying, concentrated: adopting ceramic membrane aperture is 150nm, and working pressure is 0.130Mpa, carries out purifying, concentrated to supernatant liquor with this understanding;
(E) preparation: concentrated solution is made to myrtillin leave pigment by lyophilize.
Embodiment 2
A method prepared by myrtillin leave pigment high efficiency extraction, it comprises the following steps:
(A) pulverize: taking Yixing, fresh myrtillin leave is raw material, water cleans, and then passes through mechanical disintegration, stand-by;
(B) extract: according to solid-liquid ratio 1:15(g/mL) to pulverize after myrtillin leave slag in add water, set ultrasonic-microwave-assisted and extract parameter: ultrasonic frequency is 40KHz, extract temperature 50 C, microwave power 90W, extraction time 25min carries out ultrasonic-microwave-assisted and extracts under this parameter;
(C) centrifugal: to be 9000rpm at centrifugal rotational speed, under the condition of centrifugation time 25min, to carry out frozen centrifugation, remove precipitation, get supernatant liquor stand-by;
(D) purifying, concentrated: adopting ceramic membrane aperture is 160nm, and working pressure is 0.115Mpa, carries out purifying, concentrated to supernatant liquor with this understanding;
(E) preparation: concentrated solution is made to myrtillin leave pigment by lyophilize.
Embodiment 3
A method prepared by myrtillin leave pigment high efficiency extraction, it comprises the following steps:
(A) pulverize: taking Yixing, fresh myrtillin leave is raw material, water cleans, and then passes through mechanical disintegration, stand-by;
(B) extract: according to solid-liquid ratio 1:20(g/mL) to pulverize after myrtillin leave slag in add water, set ultrasonic-microwave-assisted and extract parameter: ultrasonic frequency is 40KHz, extract 55 DEG C of temperature, microwave power 85W, extraction time 30min carries out ultrasonic-microwave-assisted and extracts under this parameter;
(C) centrifugal: to be 8000rpm at centrifugal rotational speed, under the condition of centrifugation time 30min, to carry out frozen centrifugation, remove precipitation, get supernatant liquor stand-by;
(D) purifying, concentrated: adopting ceramic membrane aperture is 180nm, and working pressure is 0.110Mpa, carries out purifying, concentrated to supernatant liquor with this understanding;
(E) preparation: concentrated solution is made to myrtillin leave pigment by lyophilize.
Embodiment 4
A method prepared by myrtillin leave pigment high efficiency extraction, it comprises the following steps:
(A) pulverize: taking Yixing, fresh myrtillin leave is raw material, water cleans, and then passes through mechanical disintegration, stand-by;
(B) extract: according to solid-liquid ratio 1:30(g/mL) to pulverize after myrtillin leave slag in add water, set ultrasonic-microwave-assisted and extract parameter: ultrasonic frequency is 40KHz, extract temperature 60 C, microwave power 75W, extraction time 40min carries out ultrasonic-microwave-assisted and extracts under this parameter;
(C) centrifugal: to be 7000rpm at centrifugal rotational speed, under the condition of centrifugation time 40min, to carry out frozen centrifugation, remove precipitation, get supernatant liquor stand-by;
(D) purifying, concentrated: adopting ceramic membrane aperture is 200nm, and working pressure is 0.095Mpa, carries out purifying, concentrated to supernatant liquor with this understanding;
(E) preparation: concentrated solution is made to myrtillin leave pigment by lyophilize.
Claims (2)
1. the method that prepared by myrtillin leave pigment high efficiency extraction, is characterized in that it comprises the following steps:
(A) pulverize: after myrtillin leave is cleaned, carry out mechanical disintegration;
(B) extract: in the myrtillin leave slag after pulverizing, add water, then carry out ultrasonic-microwave-assisted and extract;
(C) centrifugal: to adopt frozen centrifugation, remove precipitation, get supernatant liquor;
(D) purifying, concentrated: under ceramic membrane and working pressure, supernatant liquor is carried out to purifying, concentrated;
(E) preparation: concentrated solution is prepared to myrtillin leave pigment by lyophilize;
In step (B), water is as extracting solvent, and the ratio of myrtillin leave slag and water is 1:30-1:10, and unit is g/mL;
The processing parameter that ultrasonic in step (B)-microwave-assisted extracts myrtillin leave pigment is: ultrasonic frequency is 40kHz, extracts temperature 40-60 DEG C, microwave power 75-95W, extraction time 20-40min;
Described in step (D), ceramic membrane aperture is 150-200nm, and working pressure is 0.095-0.130MPa.
2. the method for preparing according to the myrtillin leave pigment high efficiency extraction described in claim l, is characterized in that the processing parameter of frozen centrifugation in step (C) is: centrifugal rotational speed is 7000-10000rpm, and centrifugation time is 20-40min.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN104479397A (en) * | 2014-10-29 | 2015-04-01 | 宁波广源纺织品有限公司 | Vaccinium bracteatum Thunb. plant dye extraction method |
| CN105369654B (en) * | 2015-11-18 | 2017-11-17 | 江阴职业技术学院 | Blueberry leaf vegetable colour is used for the dyeing of black-and-blue silk |
| CN107099167A (en) * | 2017-04-14 | 2017-08-29 | 罗莱生活科技股份有限公司 | A kind of wormwood dyestuff and its production and use |
| CN107245251A (en) * | 2017-06-07 | 2017-10-13 | 苏州大学 | A kind of preparation method and application of blueberry leaf and its extract |
| 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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