CN102850820A - Method for preparing lycium ruthenicum pigment microcapsules by using piercing method - Google Patents
Method for preparing lycium ruthenicum pigment microcapsules by using piercing method Download PDFInfo
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- CN102850820A CN102850820A CN2012103560063A CN201210356006A CN102850820A CN 102850820 A CN102850820 A CN 102850820A CN 2012103560063 A CN2012103560063 A CN 2012103560063A CN 201210356006 A CN201210356006 A CN 201210356006A CN 102850820 A CN102850820 A CN 102850820A
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Abstract
The invention discloses a method for preparing lycium ruthenicum pigment microcapsules by using a piercing method. The method comprises the following steps of using lycium ruthenicum fresh fruits or lycium ruthenicum dried fruits to serve as raw materials, crushing, conducting acidity ethanol digestion, extracting by using a microwave extractor, extracting residues for 2-3 times by using the acidity ethanol after filtering, combining an extracting solution, and conducting decompression concentration to obtain a pigment concentrated solution; and conducting adsorption, elution, desorption and decompression concentration on the pigment concentrated solution through macroporous resin, adding an embedding medium in proportion, conducting solidification, filtering, laminating, filtering and return soaking, drying under ordinary pressure at the temperature of 40-50 DEG C to obtain the lycium ruthenicum pigment microcapsules. An embedding ratio of the lycium ruthenicum pigment microcapsules prepared by the process is 70%-80%, lycium ruthenicum pigments have a slow release function after microencapsulation, more than 70% pigments can be released within 24 hours, the shape is kept to be complete, stability of the lycium ruthenicum pigment microcapsules in an 75% of relative humidity environment is obviously improved, and the weight increase of the microcapsules caused by moisture absorption is lower than 10%.
Description
Technical field
The present invention relates to adopt orifice method to prepare the method for Assessment of Pigment of Lycium ruthenicum Murr microcapsule.
Background technology
Black fruit lyceum is rich in anthocyanogen, is a kind of rare natural anthocyanin class pigment resource.The black fruit lyceum yielding ability is good, and its pigment both can dye, and certain medical health care function is also arranged.Modern medicine study proof black fruit lycium plant fruit extract has reducing blood-fat, immunomodulatory, treatment cardiovascular system diseases, arteriosclerosis, the effect such as antitumor, but the less stable of Assessment of Pigment of Lycium ruthenicum Murr, such as moisture-sensitive, easy oxidation etc. cause the pigment rate of utilization to descend.
Summary of the invention
The purpose of this invention is to provide a kind of employing cryoconcentration, the constant pressure and dry technology, the exploitation nutritive ingredient is high, has the Assessment of Pigment of Lycium ruthenicum Murr microcapsule preparation method of significantly stablizing pigment and improving the pigment anti-oxidant activity.
The present invention adopts following technical scheme:
A kind of orifice method prepares the method for Assessment of Pigment of Lycium ruthenicum Murr microcapsule, may further comprise the steps:
(1) take black fruit lyceum fresh fruit or black fruit lyceum dry fruit as raw material, broken, acidic ethanol lixiviate 12h～20h, solid-liquid ratio is 1: 20～1: 60, extract 20min～30min in the microwave extraction instrument, after the filtration residue is extracted 2-3 time with acidic ethanol again, united extraction liquid, concentrating under reduced pressure obtains pigment concentrate; Described acidic ethanol is: contain the ethanol of mass concentration 0.1%-0.3%HCl, it is the ethanol of 45%-95% that ethanol adopts concentration;
(2) with described pigment concentrate through macroporous resin adsorption, wash-out, desorb, behind the concentrating under reduced pressure, pigment concentrate and embedding medium are with 1: 1-1: 3 mass ratio stirs, be injected into 1%～5% calcium chloride solution with syringe, place under 0～4 ℃ of condition and leave standstill 0.5h～3h, then will condensing pearl, to be filled into mass percent concentration be to leave standstill 15min in 1%～3% the chitosan aqueous solution, 200 orders filter, it is to leave standstill 5min in 1%～5% the sodium alginate aqueous solution that the cohesion pearl is immersed mass percent concentration again, with in and surface charge, filter, deionized water wash, constant pressure and dry under 40 ℃～50 ℃ condition obtains the Assessment of Pigment of Lycium ruthenicum Murr microcapsule.
Described method, wherein embedding medium refers to pH to be 3.0 phosphate buffered saline buffer heating for dissolving sodium alginate, is configured to mass concentration and is 1%～5% sodium alginate soln, fully dissolving is cooled to room temperature.
Described method, described pH is that 3.0 phosphate buffered saline buffer collocation method is: the Sodium phosphate dibasic of getting 411ml concentration and be 0.2mol/L and 1589ml concentration are that the citric acid solution of 0.1mol/L mixes;
0.2mol/L Sodium phosphate dibasic: take by weighing 71.6gNa2HPO4-12H2O, be dissolved in 1000ml water;
0.2mol/L Sodium phosphate dibasic: take by weighing 35.01gNa2HPO4-2H2O, be dissolved in 1000ml water;
0.1mol/L citric acid solution: take by weighing 21.01gC4H2O7-H2O, be dissolved in 1000ml water.
A kind of Assessment of Pigment of Lycium ruthenicum Murr anti-oxidant activity of the present invention microcapsule preparation method has following beneficial effect compared with prior art:
1, because the raw material that the present invention selects is the free of contamination lycium ruthenicum fruit of pure natural, guaranteed the source of pigment safely, reliably.
2, owing to adopting solvent normal temperature and microwave-assisted lixiviate set column chromatography for separation technology that pigment is extracted, the present invention separates, whole process is carried out always at normal temperatures, therefore, not only effectively shortened and extracted the time of separating, reduced the energy consumption in the technological process, and resulting product purity is high, stable performance, the Medicines and Health Product raw material that can be applicable to the natural pigment foodstuff additive and have antioxygenation.
3, because the present invention adopts the complex coacervation gel method to prepare pigment microcapsule, operation is simple.
4, because the present invention adopts the sodium alginate-chitosan microcapsule of natural polysaccharide preparation as the carrier of pigment, have the advantages such as good biocompatibility, preparation condition gentleness and immunogenicity are low.
5, because the present invention adopts sodium alginate that pigment is carried out first embedding, the multiple film of chitosan carries out micro encapsulation to Assessment of Pigment of Lycium ruthenicum Murr, studies show that the stability through the Assessment of Pigment of Lycium ruthenicum Murr behind the micro encapsulation improves significantly, the biological activity of pigment slightly reduces before and after the microcapsule in two months, test confirms that the Assessment of Pigment of Lycium ruthenicum Murr behind the micro encapsulation has slow releasing function, can discharge pigment in the 24h more than 70%, and maintenance complete form, show that it can be used as sustained release dosage and discharges for a long time pigment, more is applicable to absorption of human body.Stability in humidity environment also is significantly improved, and in 75% relative humidity environment, the moisture absorption of microcapsule is increased weight less than 10%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
The grade estimation that embodiment 1 orifice method prepares Assessment of Pigment of Lycium ruthenicum Murr microcapsule and pigment microcapsule may further comprise the steps:
(1) with black fruit lyceum dry fruit (the perhaps real at room temperature dried and crushed of the fresh fruit of black fruit lycium plant, or 40 ℃～120 ℃ lower bakings 2～48 hours) it is carried out pulverizing after the removal of impurities, take by weighing 10g, be lixiviate 20h under 0.3% 75% the alcohol solvent normal temperature with concentration of hydrochloric acid, solid-liquid ratio is 1: 50 (v/v), then put into the microwave extraction instrument and extract 20min, microwave irradiation power is 70W, extracting solution is collected supernatant liquor after the 8000r/min whizzer filters 20min, and be that 0.3% 75% ethanolic soln extracts 3 times in the microwave extraction instrument with concentration of hydrochloric acid again with residue, each solid-liquid ratio is 1: 30 (v/v), microwave irradiation power is 70W, and the extracting solution that obtains after filtering 20min, the 8000r/min whizzer collected supernatant liquor, united extraction liquid, concentrating under reduced pressure, Recycled ethanol obtains the Assessment of Pigment of Lycium ruthenicum Murr concentrated solution.
With the concentrated solution of Assessment of Pigment of Lycium ruthenicum Murr through macroporous resin adsorption, be washed till sugar-free with deionized water, acid, be that 0.3% 75% ethanolic soln is washed resin column with hydrochloric concentration again, colourless to elutriant, with the elutriant concentrating under reduced pressure, Recycled ethanol, (pH is 3.0 phosphate buffered saline buffer heating for dissolving sodium alginate for pigment concentrate and embedding medium, be configured to mass concentration and be 2% sodium alginate soln, fully be cooled to room temperature after the dissolving and get embedding medium) stir with 1: 3 mass ratio, be 2% calcium chloride water with pigment concentrate and embedding medium mixed solution implantation quality percentage concentration with syringe, place under 3 ℃ of conditions and leave standstill 0.5h, then will condensing pearl, to be filled into mass percent concentration be to leave standstill 15min in 1% the chitosan aqueous solution, through 200 purpose filter-cloth filterings, it is to leave standstill 5min in 2% the sodium alginate aqueous solution that the cohesion pearl is immersed mass percent concentration again, with in and surface charge, through 200 purpose filter-cloth filterings, deionized water wash, constant pressure and dry under 50 ℃ condition, obtain the Assessment of Pigment of Lycium ruthenicum Murr microcapsule.
The method of Assessment of Pigment of Lycium ruthenicum Murr microcapsule grade estimation is as follows:
(1) measuring method of Assessment of Pigment of Lycium ruthenicum Murr content is:
1. prepare sample solution:
Precision takes by weighing 0.337g Assessment of Pigment of Lycium ruthenicum Murr microcapsule sample, is settled to 100mL with 75% ethanol of pH3.0, mixes, and namely is mixed with Assessment of Pigment of Lycium ruthenicum Murr microcapsule testing sample solution.
2. preparation standard curve
Precision takes by weighing Assessment of Pigment of Lycium ruthenicum Murr 0.3000g, 75% ethanol with pH3.0 is settled to 100mL, therefrom get 2,4,6,8,10,12,14mL moves into respectively in the 50mL volumetric flask, 75% ethanol with pH3.0 is settled to scale, mix, namely be mixed with concentration and be 0.12,0.24,0.36,0.48,0.60,0.72, the Assessment of Pigment of Lycium ruthenicum Murr standardized solution of 0.84mg/mL.Take 75% ethanol of pH3.0 as reference, under wavelength 525nm, record its light absorption value A with the Cary-200 ultraviolet-visible pectrophotometer, with concentration C absorbance A is returned, getting regression equation is A=0.59923 * C-0.01238, R=0.9994.
3. the content of Assessment of Pigment of Lycium ruthenicum Murr in the working sample solution
Take 75% ethanol of pH3.0 as reference, under wavelength 525nm, record the light absorption value 0.23 of Assessment of Pigment of Lycium ruthenicum Murr microcapsule testing sample solution with the Cary-200 ultraviolet-visible pectrophotometer, check in the content 0.404mg/ml of Assessment of Pigment of Lycium ruthenicum Murr, Assessment of Pigment of Lycium ruthenicum Murr content 12g/100g in the sample at typical curve.
(2) measuring method of the embedding rate of microcapsule and embedding efficiency is
1. embedding rate (%)=(add-on of Assessment of Pigment of Lycium ruthenicum Murr content/Assessment of Pigment of Lycium ruthenicum Murr * 100% in the microcapsule product, by Assessment of Pigment of Lycium ruthenicum Murr content 12g/100g in the microcapsule that record in (1), the add-on of Assessment of Pigment of Lycium ruthenicum Murr is 0.209g, and bringing the embedding rate formula into, namely to get embedding rate be 57%.
2. the gross weight of the pigment total amount/microcapsule in embedding efficiency (%)=microcapsule * 100%, by Assessment of Pigment of Lycium ruthenicum Murr content 12g/100g in the microcapsule that record in (1), the gross weight of microcapsule is 0.337g, embedding efficiency is 36%.
(3) measuring method of microcapsule release rate in the gastric juice simulated solution
At 50mL gastric juice simulated solution (the 0.01mol/LHCl solution that contains 0.09mol/LNaCl, pH2.0) add the 50g microcapsule in, under 37 ℃ condition, centrifugal with the speed that per minute 60 turns, respectively in 1h, 2h, 4h, 8h, 12h, 24h, 48h hour sampling, measuring method by (1) Assessment of Pigment of Lycium ruthenicum Murr content detects pigment content, calculates release rate according to following formula, the results are shown in Table 1.
Microcapsule weight * the drug loading of the amount of pigment that discharges in release rate (%)=gastric juice simulated solution/adding * 100%
Release rate result in the table 1 gastric juice simulated solution
As can be seen from Table 1 the release rate of pigment microcapsule in the gastric juice simulated solution in time prolongation and increase, pigment release rate within 48h is 1.38%.
(4) measuring method of microcapsule release rate in the intestinal juice simulated solution
In 50mL intestinal juice simulated solution (phosphoric acid buffer that contains the 29mmol/LpH7.4 of 76.5mmol/NaCl), add the 50g microcapsule, under 37 ℃ condition, centrifugal with the speed that per minute 60 turns, respectively in 1h, 2h, 4h, 8h, 12h, 24h, 48h hour sampling, measuring method by (1) Assessment of Pigment of Lycium ruthenicum Murr content detects pigment content, calculate release rate according to following formula, the results are shown in Table 2.
Microcapsule weight * the drug loading of the amount of pigment that discharges in release rate (%)=intestinal juice simulated solution/adding * 100%
Release rate result in the table 2 intestinal juice simulated solution
As can be seen from Table 2 the release rate of pigment microcapsule in the intestinal juice simulated solution in time prolongation and increase, pigment release rate within 48h is 0.64%.
(5) Assessment of Pigment of Lycium ruthenicum Murr microcapsule wet fastness measuring method
Getting pigment microcapsule 54g places test tube to put into the brown wide-necked bottle of sealing, place 25 ℃, in the environment of relative humidity 75%, respectively at the 5th, 10,15 day mensuration pigment content (measuring method by (1) Assessment of Pigment of Lycium ruthenicum Murr content detects pigment content), it the results are shown in Table 3.
Table 3 humidity test
The Assessment of Pigment of Lycium ruthenicum Murr microcapsule are under 75% relative humidity condition, and the moisture absorption of microcapsule weightening finish is about 7%, meets the manufacture requirement.
2 one kinds of Assessment of Pigment of Lycium ruthenicum Murr anti-oxidant activities of embodiment microcapsule preparation method may further comprise the steps:
(1) the black fruit lyceum dry fruit is carried out pulverizing after the removal of impurities to it, take by weighing 10g, with lixiviate 12h under 95% the alcohol solvent normal temperature that contains 0.1%HCl, solid-liquid ratio is 1: 30, then put into the microwave extraction instrument and extract 15min, microwave irradiation power is 80W, extracting solution is collected supernatant liquor after the 6000r/min whizzer filters 15min, and residue extracted 2 times in the microwave extraction instrument with 95% the ethanolic soln that contains 0.1%HCl again, each solid-liquid ratio is 1: 30, microwave irradiation power is 80W, and the extracting solution that obtains after filtering 15min, the 6000r/min whizzer collected supernatant liquor, united extraction liquid, concentrating under reduced pressure, Recycled ethanol obtains the Assessment of Pigment of Lycium ruthenicum Murr concentrated solution.
With the concentrated solution of Assessment of Pigment of Lycium ruthenicum Murr through macroporous resin adsorption, be washed till sugar-free with deionized water, acid, wash resin column through 95% the ethanolic soln that contains 0.1%HCl again, colourless to elutriant, with the elutriant concentrating under reduced pressure, obtain pigment concentrate, pigment concentrate and 2% sodium alginate to embed agent stir with 1: 1 ratio, be injected into 3% calcium chloride solution with syringe, place under 4 ℃ of conditions and leave standstill 0.5h, then will coagulate pearl and be filled in 2% the chitosan solution and leave standstill 15min, through 200 purpose filter-cloth filterings, the cohesion pearl immersed in 2% the calcium chloride solution again leaves standstill 5min, with in and surface charge, through 200 purpose filter-cloth filterings, deionized water wash, constant pressure and dry under 50 ℃ condition obtains the Assessment of Pigment of Lycium ruthenicum Murr microcapsule, and the embedding rate of Assessment of Pigment of Lycium ruthenicum Murr microcapsule is 75% after measured.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (3)
1. an orifice method prepares the method for Assessment of Pigment of Lycium ruthenicum Murr microcapsule, it is characterized in that, may further comprise the steps:
(1) take black fruit lyceum fresh fruit or black fruit lyceum dry fruit as raw material, broken, acidic ethanol lixiviate 12h～20h, solid-liquid ratio is 1: 20～1: 60, extract 20min～30min in the microwave extraction instrument, after the filtration residue is extracted 2-3 time with acidic ethanol again, united extraction liquid, concentrating under reduced pressure obtains pigment concentrate; Described acidic ethanol is: contain the ethanol of mass concentration 0.1%-0.3%HCl, it is the ethanol of 45%-95% that ethanol adopts concentration;
(2) with described pigment concentrate through macroporous resin adsorption, wash-out, desorb, behind the concentrating under reduced pressure, pigment concentrate and embedding medium are with 1: 1-1: 3 mass ratio stirs, be injected into 1%～5% calcium chloride solution with syringe, place under 0～4 ℃ of condition and leave standstill 0.5h～3h, then will condensing pearl, to be filled into mass percent concentration be to leave standstill 15min in 1%～3% the chitosan aqueous solution, 200 orders filter, it is to leave standstill 5min in 1%～5% the sodium alginate aqueous solution that the cohesion pearl is immersed mass percent concentration again, with in and surface charge, filter, deionized water wash, constant pressure and dry under 40 ℃～50 ℃ condition obtains the Assessment of Pigment of Lycium ruthenicum Murr microcapsule.
2. method according to claim 1 is characterized in that, wherein embedding medium refers to pH to be 3.0 phosphate buffered saline buffer heating for dissolving sodium alginate, is configured to mass concentration and is 1%～5% sodium alginate soln, and fully dissolving is cooled to room temperature.
3. method according to claim 2, described pH is that 3.0 phosphate buffered saline buffer collocation method is: the Sodium phosphate dibasic of getting 411ml concentration and be 0.2mol/L and 1589ml concentration are that the citric acid solution of 0.1mol/L mixes;
0.2mol/L Sodium phosphate dibasic: take by weighing 71.6gNa2HPO4-12H2O, be dissolved in 1000ml water;
0.2mol/L Sodium phosphate dibasic: take by weighing 35.01gNa2HPO4-2H2O, be dissolved in 1000ml water;
0.1mol/L citric acid solution: take by weighing 21.01gC4H2O7-H2O, be dissolved in 1000ml water.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103230473A (en) * | 2013-02-28 | 2013-08-07 | 上海基赛生物医药科技有限公司 | Lycium ruthenicum Murr effective extract and its extraction method and use |
| CN104248036A (en) * | 2014-09-19 | 2014-12-31 | 青海诺蓝杞生物科技开发有限公司 | Lycium ruthenicum Murr procyanidine effervescent tablet and production method thereof |
| CN105079281A (en) * | 2015-09-07 | 2015-11-25 | 中国科学院西北高原生物研究所 | Lycium ruthenicum anthocyanin crude extract and controlled-release microcapsule thereof |
| CN105238098A (en) * | 2015-11-02 | 2016-01-13 | 江苏食品药品职业技术学院 | Dynamic gradient embedding method for purple corn cob anthocyanin |
| CN107198240A (en) * | 2017-07-12 | 2017-09-26 | 青岛大学 | The combined extraction method of plurality of active ingredients in black fruit fructus lycii |
| WO2017205173A1 (en) * | 2016-05-24 | 2017-11-30 | Ohio State Innovation Foundation | Uses of acylated anthocyanins extracted from black goji (lycium ruthenicum murr.) as a source of natural color |
| CN107467482A (en) * | 2017-08-25 | 2017-12-15 | 江苏食品药品职业技术学院 | A kind of solid dispersions of fat-soluble wolfberry pigment and the application in terms of food and health products |
| CN107568745A (en) * | 2016-11-21 | 2018-01-12 | 广西大学 | A kind of method that orifice method prepares the anti-oxidant titanium microcapsules of rice |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230473A (en) * | 2013-02-28 | 2013-08-07 | 上海基赛生物医药科技有限公司 | Lycium ruthenicum Murr effective extract and its extraction method and use |
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| CN104248036A (en) * | 2014-09-19 | 2014-12-31 | 青海诺蓝杞生物科技开发有限公司 | Lycium ruthenicum Murr procyanidine effervescent tablet and production method thereof |
| CN105079281A (en) * | 2015-09-07 | 2015-11-25 | 中国科学院西北高原生物研究所 | Lycium ruthenicum anthocyanin crude extract and controlled-release microcapsule thereof |
| CN105238098A (en) * | 2015-11-02 | 2016-01-13 | 江苏食品药品职业技术学院 | Dynamic gradient embedding method for purple corn cob anthocyanin |
| WO2017205173A1 (en) * | 2016-05-24 | 2017-11-30 | Ohio State Innovation Foundation | Uses of acylated anthocyanins extracted from black goji (lycium ruthenicum murr.) as a source of natural color |
| CN107568745A (en) * | 2016-11-21 | 2018-01-12 | 广西大学 | A kind of method that orifice method prepares the anti-oxidant titanium microcapsules of rice |
| CN107198240A (en) * | 2017-07-12 | 2017-09-26 | 青岛大学 | The combined extraction method of plurality of active ingredients in black fruit fructus lycii |
| CN107467482A (en) * | 2017-08-25 | 2017-12-15 | 江苏食品药品职业技术学院 | A kind of solid dispersions of fat-soluble wolfberry pigment and the application in terms of food and health products |
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