CN101843571B - Multiple emulsion for loading tea polyphenol and preparation method thereof - Google Patents

Multiple emulsion for loading tea polyphenol and preparation method thereof Download PDF

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CN101843571B
CN101843571B CN2010101512723A CN201010151272A CN101843571B CN 101843571 B CN101843571 B CN 101843571B CN 2010101512723 A CN2010101512723 A CN 2010101512723A CN 201010151272 A CN201010151272 A CN 201010151272A CN 101843571 B CN101843571 B CN 101843571B
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tea polyphenols
multiple emulsion
emulsion
sucrose ester
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CN101843571A (en
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夏强
徐峰
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Proya Cosmetics Co Ltd
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SUZHOU NANOHEALTH BIOTECH CO Ltd
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Abstract

The invention discloses a multiple emulsion for loading tea polyphenol and a preparation method thereof. The multiple emulsion comprises the following components by weight ratio: 0.5 -8 percent of tea polyphenol, 5 -15 percent of emulsifier, 10 -30 percent of lipid material and the balance of water. The emulsion has high stability, does not delaminate after being preserved for more than six months at normal temperature, does not delaminate under the condition of high-speed centrifugation at 4000r/min for 15min and can be applied to food, medicines and cosmetics.

Description

Multiple emulsion of loading tea polyphenol and preparation method thereof
Technical field
The present invention relates to a kind of preparation technique of tea polyphenols; Be specifically related to multiple emulsion carrier of a kind of supported active composition tea polyphenols and preparation method thereof; Being particularly related to a kind of is the method for preparing of the micron-sized multiple emulsion of active component with the tea polyphenols, belongs to cosmetics and technical field of food preparation.
Background technology
Tea polyphenols (Tea Polyphenols is called for short TP), another name: tea polyphenols, tea tannin are the general names of the chemical compound of catechin in the Folium Camelliae sinensis, acetone class, phenolic acids and anthocyan polyhydroxy phenols.Tea polyphenols mainly acts on: 1, remove reactive oxygen free radical, blocking-up lipid peroxidation process improves the activity of human body endoenzyme, thereby plays the effect of mutation, anticancer disease.2, prevent and treat the disease that hyperlipemia causes: 1. strengthen blood capillary obdurability, blood fat reducing, prevention liver and crown atherosclerosis; Tea polyphenols mainly shows as through the content of high density lipoprotein increasing cholesterol (HDL-C) the effect of serum cholesterol and removes accumulating of cholesterol on the arterial blood tube wall; Suppress the picked-up of cell simultaneously to low-density lipoprotein cholesterol (LDL-C); Thereby realization blood fat reducing, prevention and alleviation atherosclerosis purpose.2. blood pressure lowering: tea polyphenols has the effect of stronger inhibition conversion enzymatic activity, thereby can play the effect that reduces or keep blood pressure stabilization.3. blood sugar lowering: tea polyphenols has regulating action to the metabolism obstacles of blood glucose of human body, the blood sugar lowering level, thus effectively prevent and treat diabetes.4. prevent apoplexy: the effect that tea polyphenols has the containment lipid peroxide to produce, the elasticity of maintenance blood vessel wall makes the lax elimination of blood vessel wall vasospasm, increases the effective diameter of blood vessel, makes blood pressure drops through vasodilation, thereby prevents apoplexy effectively.5. antithrombotic: tea polyphenols has protection and repair to ED, and is prone to form complex with thrombin, and the prevention Fibrinogen becomes fibrin.In addition, tea polyphenols can effectively suppress the rising of cholesterol level in blood plasma and the liver, promotes lipid and bile acid to excrete, thus the effectively formation of anti-tampon.Existing blood fat reducing thromboembolism preventing medicine has certain toxic and side effects more and is difficult for taking for a long time.Tea polyphenols is the natural component that has the effect of blood fat reducing thromboembolism preventing in the Folium Camelliae sinensis, adds the anti-oxidation characteristics that himself has, and makes it become a kind of novel functional health product.3, improve the effect of the comprehensive immunocompetence of human body: 1. tea polyphenols stimulates the variation of antibody activity through improving the human immunoglobulin total amount and making it maintain high level, thereby improves people's overall immune ability.And can promote self conditioning functions of human body.Tea polyphenols is through regulating the amount and the activity of immunoglobulin, and realize suppressing or killing the effect confirmation of medical experiment of various pathogen, pathogenic bacteria and virus indirectly: tea polyphenols can suppress and kill bacterial infections such as streptococcus, typhoid fever bacterium, bordetella pertussis, Diplococcus pneumoniae, dysentery bacterium, staphylococcus; Suppress or reduce the virulence of diphtheria toxin, diphtherotoxin, tetanus toxin; Poliomyelitis virus, influenza virus, mumps virus, Measles virus, herpesvirus, HIV etc. are to the injury of human body; Suppress treponema pallidum and Candida albicans infecting to the people; The resisting rheumatoid disease factor etc.2. antiallergic action and skin allergy; The allergy reflection that tea polyphenols inhibition active factors such as antibody, epinephrine, enzyme etc. cause has significant curative effect to anaphylaxis diseases such as asthma.The release action of tea polyphenols ability exhibited strong inhibition histamine, the strong 2-10 of inhibition effect of the antiallergic agent that experiment proof tea polyphenols antiallergic action and anti-skin allergy ratio are used always at present doubly.3. releive the intestines and stomach anxiety, anti-scorching antidiarrheal and diuresis; Tea polyphenols has the reaction of stimulating gastrointestinal road, quickens intestinal peristalsis to reach the effect of treatment constipation.Tea polyphenols suppresses and kills to cause the various harmful pathogenetic bacterias of diarrheal through improving the comprehensive immunocompetence of human body, and the tense situation of the intestines and stomach of releiving, to reach antiinflammatory antidiarrheal effect.Flavanols compounds can the stimulation of renal vasodilation in the tea polyphenols, increases the blood flow of kidney, thereby increases the filtration rate of glomerule, makes the lactic acid in the urine obtain to get rid of.Lactic acid in human muscle, the tissue is a kind of tired material, and excreting of lactic acid can make tired human body obtain to recover.4. promote ascorbic absorption, prevent and treat vitamin C deficiency; Improve the absorption of human body for ferro, effectively prevent anemia.
Tea polyphenols is a kind of water miscible material, yet its stabilization ratio in water is relatively poor.It is perishable to meet highly basic, strong acid, illumination, hyperpyrexia and transition metal.The upper limit temperature of heat tolerance can reach about 250 ℃ in 1 and a half hours, and under ferric ion, was prone to decompose.These character owing to tea polyphenols in the prior art cause it narrower in scope of using, and effect is not obvious.Multiple emulsion is to comprise a kind of complicated emulsion system of more droplet in addition in the dispersed phase drop again, and two types of W/O/W and O/W/O are generally arranged.With W/O/W is example; Have interior water, oil phase and outer water three-phase; And at profit, water oil interface formation interfacial film; Different deliquescent materials can load on not in the homophase, can play effects such as isolation, protection, slow release, controlled-release target controlled release, and multiple emulsion is widely used in industries such as cosmetics, food, medicine.But multiple emulsion is a kind of system of complicacy, and extremely unstable, this also becomes the principal element that limits its large-scale application.Also do not have the research of the multiple emulsion of tea polyphenols in the prior art, the present invention comes therefrom.
Summary of the invention
The object of the invention is to provide a kind of multiple emulsion of loading tea polyphenol, has solved that tea polyphenol preparation stability is not good in the prior art, effect is bad, be difficult to keep problems such as long period.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of multiple emulsion of loading tea polyphenol is characterized in that said multiple emulsion comprises in the weight ratio of its component in emulsion:
Tea polyphenols 0.5%~8%;
Emulsifying agent 5%~15%;
Matrix material 10%~30%;
All the other are water.
Preferably, said multiple emulsion comprises in the weight ratio of its component in emulsion:
Tea polyphenols 0.5%~5%;
Emulsifying agent 7%~12%;
Matrix material 13%~20%;
All the other are water.
Preferably, described emulsifying agent is a hydrophilic emulsifier, is selected to gather in tristerin, fatty acid glyceride, phospholipid, tween, span and the sucrose ester one or more.
Preferably, described matrix material is selected from one or more of soybean oil, Semen Maydis oil, camellia seed oil, canola oil, Oleum Helianthi.
Another object of the present invention is to provide a kind of method for preparing of multiple emulsion of loading tea polyphenol, it is characterized in that said method comprising the steps of:
(1) prepares the aqueous solution of liquid oil phase and tea polyphenols respectively, the aqueous solution of tea polyphenols is added in the liquid oil phase and through high pressure homogenization method prepares water in oil colostrum;
(2) preparation contains the outer water of emulsifying agent; The colostrum that under 60 ℃~75 ℃, step (1) is obtained is added to the outer aqueous phase that contains emulsifying agent; And the even 1~5min of high speed shear while adding, rotating speed is controlled at 300r/min~3000r/min, obtains the multiple emulsion of loading tea polyphenol.
Preferably, the method for the liquid oil phase of preparation comprises that respectively the weighing mass ratio is the emulsifying agent and the matrix material of (1: 1)~(1: 3) in the said method, with emulsifying agent and matrix material mixing post-heating to 60 ℃~75 ℃, obtains the step of liquid oil phase after the fusion.
Preferably, the method for aqueous solution of preparation tea polyphenols comprises the weighing tea polyphenols in the said method, is dissolved in 60 ℃~75 ℃ the water, and wherein the mass ratio of tea polyphenols and water is (1: 2)~(1: 59), obtains the step of the aqueous solution of tea polyphenols.
Preferably; The method for preparing the outer water that contains emulsifying agent in the said method comprises that the weighing mass ratio is the emulsifying agent and the water of (1: 99)~(3: 47) respectively; With mixed solution being heated to 60 ℃~75 ℃, the step of the outer water that contains emulsifying agent that obtains after emulsifying agent and the water mixing.
Preferably, said method mesohigh homogenizing method may further comprise the steps:
A, 60 ℃~75 ℃ tea polyphenols aqueous solutions are joined in the liquid oil phase, rotating speed is controlled at and carries out high speed shear under 8000~12000r/min and obtained uniform emulsion in even 1~5 minute;
B, the emulsion that steps A is obtained are put into high pressure homogenizer and are circulated 3~5 times, and the control temperature is in 60 ℃~75 ℃, and pressure obtains water in oil colostrum at 300~600pa.
Preferably, the matrix material described in the said method is a kind of or this mixture of two kinds of soybean oil, Semen Maydis oil, camellia seed oil, canola oil, Oleum Helianthi.Emulsifying agent of the present invention is one or more in polyglyceryl fatty acid ester, phospholipid, tween, span and the sucrose ester.
More detailed, the method for preparing of the W/O/W multiple emulsion of loading tea polyphenol of the present invention is following:
Respectively weighing emulsifying agent and matrix material, both mass ratioes are 1: 1~1: 3, and emulsifying agent and matrix material mixing post-heating to design temperature t, t=60-75 ℃, are obtained liquid oil phase after the fusion;
Weighing tea polyphenols (TP), tea polyphenols is 0.5 with the mass ratio of outer water: 29.5-10: 20, water is heated to design temperature t, t=60-75 ℃, (TP) is soluble in water for tea polyphenols, obtains the aqueous solution of tea polyphenols;
Respectively weighing emulsifying agent and outer water, both mass ratioes are 0.5: 49.5-3: 47, with emulsifying agent and outer water mixing post-heating to design temperature t, t=60-75 ℃;
To join with the tea polyphenols aqueous solution of design temperature t uniform temp in the system in the step 1; High speed shear is even; Rotating speed is 8000~12000r/min; Shear and obtained uniform emulsion in 1~5 minute, then the emulsion that obtains being joined design temperature is that t, setting pressure are to circulate 3~5 times in the high pressure homogenizer of 600bar, obtains colostrum;
Under design temperature t, the colostrum that obtains is joined the outer aqueous phase that contains emulsifying agent, shear with high-speed shearing machine on the limit, and the limit adds, and rotating speed is 300r/min~3000r/min, and 1~5min obtains the multiple emulsion of loading tea polyphenol.
Advantage of the present invention is:
1. preparation process condition is controlled.Can be through regulating, it is 0.5%~5% tea polyphenols multiple emulsion that the rotating speed of high speed shear, high pressure homogenize cycle-index, each component ratio can be prepared content.
2. the multiple emulsion of preparation stability is better, and room temperature is preserved not stratified more than 6 months, and high speed centrifugation 4000r/min is not stratified under the condition of 15min.
3. multiple emulsion can be good at protecting the activity of tea polyphenols, plays the effect of slow release.
4. method for preparing is simple, good reproducibility.
The multiple emulsion of the W/O/W type of loading tea polyphenol of the present invention, its stability is high, and the multiple emulsion of this loading tea polyphenol can be applicable in the food and medicine cosmetics.The method for preparing of the multiple emulsion of this loading tea polyphenol is a two-step method in addition, and wherein preparation condition can be controlled, and helps suitability for industrialized production.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Fig. 1 is the method for preparing flow chart of the W/O/W type multiple emulsion of loading tea polyphenol of the present invention.
The specific embodiment
Below in conjunction with specific embodiment such scheme is further specified.Should be understood that these embodiment are used to the present invention is described and are not limited to limit scope of the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
The preparation of the W/O/W type multiple emulsion of embodiment 1 loading tea polyphenol
Pharmaceutical formulation:
Composition weight
Tea polyphenols 0.5g
Sucrose ester 1g
Fabaceous lecithin 6.25g
Soybean oil 16.25
Glyceryl monostearate 2.5g
Water 73.5g
Method for preparing:
As shown in Figure 1, take by weighing 1 gram tea polyphenols, 24.5 gram water deionized waters are heated to design temperature t=65 ℃ to deionized water, then adding tea polyphenols; Take by weighing 6.25 gram fabaceous lecithins, 2.5 gram glyceryl monostearates (GMS), soybean oil 16.25 gram mixes and is heated to 65 ℃;
Keep 65 ℃ of constant temperature, the tea polyphenols aqueous solution that step 1 is obtained joins in the oil phase that step 2 obtains, and under 10000r/min, shears with high-speed shearing machine, and the time is 1 minute, obtains more uniform emulsion; Emulsion is joined homogenizing in the high pressure homogenizer, and condition is 600bar, and 5 circulations make colostrum;
Take by weighing 1 gram sucrose ester, 49 gram deionized waters join sucrose ester in the deionized water, are heated to 65 ℃, obtain containing the outer water of sucrose ester; The above-mentioned colostrum for preparing is joined the outer aqueous phase that contains sucrose ester, disperse with high-speed shearing machine, rotating speed is 600r/min, and the time is 5min, makes the W/O/W type multiple emulsion of loading tea polyphenol;
The multiple emulsion that obtains is at 4000r/min, under the centrifugal condition of 15min, high speed centrifugation, not stratified, room temperature place 6 months not stratified.
The preparation of the W/O/W type multiple emulsion of embodiment 2 loading tea polyphenols
Pharmaceutical formulation:
Composition weight
Tea polyphenols 1g
Sucrose ester 1g
Fabaceous lecithin 6.25g
Canola oil 16.25g
Glyceryl monostearate 2.5g
Water 73g
Method for preparing:
Take by weighing 1 gram tea polyphenols, 24 gram water deionized waters are heated to design temperature t=63 ℃ to deionized water, then adding tea polyphenols; Take by weighing 6.25 gram fabaceous lecithins, 2.5 gram glyceryl monostearates (GMS), canola oil 16.25 gram mixes and is heated to 65 ℃;
Keep 65 ℃ of constant temperature, the tea polyphenols aqueous solution that step 1 is obtained joins in the oil phase that step 2 obtains, and under 10000r/min, shears with high-speed shearing machine, and the time is 1 minute, obtains more uniform emulsion; Emulsion is joined homogenizing in the high pressure homogenizer, and condition is 600bar, and 5 circulations make colostrum;
Take by weighing 1 gram sucrose ester, 49 gram deionized waters join sucrose ester in the deionized water, are heated to 65 ℃, obtain containing the outer water of sucrose ester; Colostrum is joined the outer aqueous phase that contains sucrose ester, disperse with high-speed shearing machine, rotating speed is 600r/min, and the time is 5min, makes the W/O/W type multiple emulsion of loading tea polyphenol;
The multiple emulsion that obtains is at 4000r/min, under the centrifugal condition of 15min, high speed centrifugation, not stratified, room temperature place 6 months not stratified.
The preparation of the W/O/W type multiple emulsion of embodiment 3 loading tea polyphenols
Pharmaceutical formulation:
Composition weight
Tea polyphenols 1.5g
Sucrose ester 1g
Fabaceous lecithin 7.5g
Oleum Helianthi 19.5g
Glyceryl monostearate 3g
Water 67.5g
Method for preparing:
Take by weighing 1.5 gram tea polyphenols, 18.5 gram water deionized waters are heated to design temperature t=65 ℃ to deionized water, then adding tea polyphenols; Take by weighing 7.5 gram fabaceous lecithins, 3 gram glyceryl monostearates (GMS), Oleum Helianthi 19.5 gram mixes and is heated to 65 ℃;
Keep 65 ℃ of constant temperature, the tea polyphenols aqueous solution that step 1 is obtained joins in the oil phase that step 2 obtains, and under 10000r/min, shears with high-speed shearing machine, and the time is 1 minute, obtains more uniform emulsion; Emulsion is joined homogenizing in the high pressure homogenizer, and condition is 600bar, and 5 circulations make colostrum;
Take by weighing 1 gram sucrose ester, 49 gram deionized waters join sucrose ester in the deionized water, are heated to 65 ℃, obtain containing the outer water of sucrose ester; Colostrum is joined the outer aqueous phase that contains sucrose ester, disperse with high-speed shearing machine, rotating speed is 600r/min, and the time is 5min, makes the W/O/W type multiple emulsion of loading tea polyphenol;
The multiple emulsion that obtains is at 4000r/min, under the centrifugal condition of 15min, high speed centrifugation, not stratified, room temperature place 6 months not stratified.
The preparation of the W/O/W type multiple emulsion of embodiment 4 loading tea polyphenols
Pharmaceutical formulation:
Composition weight
Tea polyphenols 1g
Tween 80 1g
Fabaceous lecithin 5g
Camellia seed oil 13g
Sorbester p17 2g
Water 78g
Method for preparing:
Take by weighing 1 gram tea polyphenols, 29 gram water deionized waters are heated to design temperature t=65 ℃ to deionized water, then adding tea polyphenols; Take by weighing 5 gram fabaceous lecithins, 2 gram sorbester p17s (Span 80), camellia seed oil 13 gram mixes and is heated to 65 ℃;
Keep 65 ℃ of constant temperature, the tea polyphenols aqueous solution that step 1 is obtained joins in the oil phase that step 2 obtains, and under 10000r/min, shears with high-speed shearing machine, and the time is 1 minute, obtains more uniform emulsion; Emulsion is joined homogenizing in the high pressure homogenizer, and condition is 600bar, and 5 circulations make colostrum;
Take by weighing 1 gram tween 80 (TWEEN 80), 49 gram deionized waters join sucrose ester in the deionized water, are heated to 65 ℃, obtain containing the outer water of sucrose ester; Colostrum is joined the outer aqueous phase that contains sucrose ester, disperse with high-speed shearing machine, rotating speed is 600r/min, and the time is 5min, makes the W/O/W type multiple emulsion of loading tea polyphenol;
The multiple emulsion that obtains is at 4000r/min, under the centrifugal condition of 15min, high speed centrifugation, not stratified, room temperature place 6 months not stratified, the multiple emulsion of the loading tea polyphenol that obtains can be used for preparing cosmetics, food.
Above-mentioned instance only is explanation technical conceive of the present invention and characteristics, and its purpose is to let the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.

Claims (2)

1. the multiple emulsion of a loading tea polyphenol is characterized in that said multiple emulsion is the W/O/W multiple emulsion; Said multiple emulsion is counted with the weight ratio of its component in emulsion:
Tea polyphenols 1g;
Sucrose ester 1g;
Fabaceous lecithin 6.25g;
Canola oil 16.25g;
Glyceryl monostearate 2.5g;
Water 73g;
Said multiple emulsion prepares through following method:
(1) take by weighing 1 gram tea polyphenols, 24 gram deionized waters are heated to design temperature t=63 ℃ to deionized water, add tea polyphenols then, obtain the aqueous solution of tea polyphenols;
(2) take by weighing 6.25 gram fabaceous lecithins, 2.5 gram glyceryl monostearates (GMS), canola oil 16.25 grams mix and are heated to 65 ℃ obtaining oil phase;
(3) keep 65 ℃ of constant temperature, the tea polyphenols aqueous solution that step 1 is obtained joins in the oil phase that step 2 obtains, and under 10000r/min, shears with high-speed shearing machine, and the time is 1 minute, obtains emulsion; Emulsion is joined homogenizing in the high pressure homogenizer, and condition is 600bar, and 5 circulations make colostrum;
(4) take by weighing 1 gram sucrose ester, 49 gram deionized waters join sucrose ester in the deionized water, are heated to 65 ℃, obtain containing the outer water of sucrose ester; Colostrum is joined the outer aqueous phase that contains sucrose ester, disperse with high-speed shearing machine, rotating speed is 600r/min, and the time is 5min, makes the W/O/W type multiple emulsion of loading tea polyphenol.
2. the multiple emulsion of a loading tea polyphenol is characterized in that said multiple emulsion is the W/O/W multiple emulsion; Said multiple emulsion is counted with the weight ratio of its component in emulsion:
Tea polyphenols 1.5g;
Sucrose ester 1g;
Fabaceous lecithin 7.5g;
Oleum Helianthi 19.5g;
Glyceryl monostearate 3g;
Water 67.5g;
Said multiple emulsion prepares through following method:
(1) take by weighing 1.5 gram tea polyphenols, 18.5 gram deionized waters are heated to design temperature t=65 ℃ to deionized water, add tea polyphenols then, obtain the aqueous solution of tea polyphenols;
(2) take by weighing 7.5 gram fabaceous lecithins, 3 gram glyceryl monostearates (GMS), Oleum Helianthi 19.5 grams mix and are heated to 65 ℃ obtaining oil phase;
(3) keep 65 ℃ of constant temperature, the tea polyphenols aqueous solution that step 1 is obtained joins in the oil phase that step 2 obtains, and under 10000r/min, shears with high-speed shearing machine, and the time is 1 minute, obtains emulsion; Emulsion is joined homogenizing in the high pressure homogenizer, and condition is 600bar, and 5 circulations make colostrum;
(4) take by weighing 1 gram sucrose ester, 49 gram deionized waters join sucrose ester in the deionized water, are heated to 65 ℃, obtain containing the outer water of sucrose ester; Colostrum is joined the outer aqueous phase that contains sucrose ester, disperse with high-speed shearing machine, rotating speed is 600r/min, and the time is 5min, makes the W/O/W type multiple emulsion of loading tea polyphenol.
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CN103976901A (en) * 2014-05-22 2014-08-13 东南大学 Coenzyme Q10 and tea polyphenol loaded micro-nano carrier, as well as preparation and application methods thereof
CN104305320B (en) * 2014-10-24 2016-07-13 南京农业大学 A kind of processing method of green tea sausage
CN105342866A (en) * 2015-10-21 2016-02-24 苏州纳康生物科技有限公司 Green tea extract nanostructured lipid carrier and preparation method thereof
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CN107811055A (en) * 2017-11-16 2018-03-20 合肥工业大学 A kind of pickering emulsions and preparation method based on ethyl cellulose and camellia seed oil
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