CN107581343A - A kind of preparation method of LBP-X particle - Google Patents
A kind of preparation method of LBP-X particle Download PDFInfo
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- CN107581343A CN107581343A CN201711034846.7A CN201711034846A CN107581343A CN 107581343 A CN107581343 A CN 107581343A CN 201711034846 A CN201711034846 A CN 201711034846A CN 107581343 A CN107581343 A CN 107581343A
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Abstract
The invention discloses a kind of preparation method of LBP-X particle, carry out in accordance with the following steps：Matrimony vine is soaked 30~35min by step 1), is then beaten with beater, matrimony vine slurries are obtained with filtered through gauze；Step 2) adds enzyme in distilled water, and 30~35min is activated between 30~35 DEG C, obtains enzyme mixation；Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value, is progressively warming up to 90 DEG C, 30~35min of enzyme deactivation, is cooled to room temperature, filters, and stands, takes supernatant, produce polysaccharide solution.Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol precipitation, distilled water washs repeatedly, dry Lycium barbarum polysaccharide extract.The Lycium barbarum polysaccharide extract that step 5) obtains step, maltodextrin, Icing Sugar are added, addition ethanol is wetting agent softwood, then particle is made, and crosses 12~16 mesh sieves, drying to obtain product.
Description
Technical field
The invention belongs to technical field of health care food, and in particular to a kind of preparation method of LBP-X particle.
Background technology
LBP-X is a kind of bioactive substance extracted from matrimony vine, has and promotes T, B, CTL, NK and macrophage
Etc. immunologic function, the cell factors such as IL-2, IL-3 and TNF β are promoted to produce.LBP-X be matrimony vine pulp most effective composition it
One, it is where the elite of matrimony vine, easily absorbs.With reducing blood lipid, lipotropy, there is antitumor action, there is anti-aging
Effect, immune and immunoloregulation function can be strengthened, the effect of hematopoiesis function can be promoted.
Granule, mean that the extract of medicine or medicinal material is made with certain particle size with suitable auxiliary material or fine medicinal material powder
The preparation of dry particle shape, or bulk is pressed into single dose particle, the used time is taken after mixing it with water with boiling water, therefore also known as " electuary ".
Granule is one of wide formulation of clinical practice, its feature：1. compared with powder, the dispersiveness of granule,
Tack, aggregation, hygroscopicity are smaller, are advantageous to divided dose；2. Chinese herbal granules are in traditional decoction and syrup
On the basis of the formulation that develops, both maintained the advantages of decoction effect is rapid, and overcome the trouble that decocts temporarily again and easily mould bad become
The shortcomings that matter；3. granule can dissolve or be suspended in water, be advantageous to medicine and absorb in vivo, it is rapid-action to maintain liquid preparation
The characteristics of, but it is stable compared with liquid preparation property, it is easy to take, carries, stores；4. it is suitably added aromatic, flavouring, colouring agent
Deng can be made into the various pharmaceutical preparation of color, patient is happy to take, to particularly suitable (some granule sugar contents of children
It is higher, the elderly and diabetic are not applied to, have the granule of sugar-free at present)；5. granule also has deficiency, due to
Grain is not of uniform size, is not easy accurately with volumetric method divided dose, and particularly several relative densities are different, the particle of quantity not etc. mixes
When, also have that mixed performance is poor, the easy phenomenon being layered.
The content of the invention
Goal of the invention：For weak point of the prior art, the invention provides a kind of preparation of LBP-X particle
Method.
Technical scheme：The preparation method of LBP-X particle of the present invention, is carried out in accordance with the following steps：
Matrimony vine is soaked 30~35min by step 1), is then beaten with beater, wolfberry fruit syrup is obtained with filtered through gauze
Liquid；
Step 2) adds enzyme in distilled water, and 30~35min is activated between 30~35 DEG C, obtains enzyme mixation；
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
90 DEG C are progressively warming up to, 30~35min of enzyme deactivation, is cooled to room temperature, is filtered, is stood, is taken supernatant, produce polysaccharide solution.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol precipitation, distilled water washs repeatedly, dry LBP-X extraction
Thing.
The Lycium barbarum polysaccharide extract that step 5) obtains step, maltodextrin, Icing Sugar are added, addition ethanol is wetting agent system
Softwood, then particle is made, cross 12~16 mesh sieves, drying to obtain product.
Specifically, the enzyme described in step 2) is amylase, one kind in cellulase；The addition of enzyme is matrimony vine slurries matter
The 0.5~0.6% of amount.
Specifically, the regulation acid-base value in step 3) is that pH value is adjusted into 7.5.
Specifically, the concentration of ethanol is 95% in step 4).
Specifically, the concentration of ethanol is 80% in step 5)；Raw material mass mixture ratio in step 5) is：LBP-X extracts
2 parts of thing, 5~8 parts of dextrin, 5~8 parts of Icing Sugar.
It has been surprisingly found that carried out during such as softwood processed of step 5) in negative pressure, then the particle of granulation is big
It is small more uniform, and the distribution of active component is also more uniform, and the divided dose for being advantageous to medicament uses.Further research
It was found that when pressure is -1~-0.5mpa, the most properly.It is further to also found, if when particle is made, make entirely mistake
If journey is carried out in the hot-air of flowing, its effect is more preferable, can not only save follow-up drying link, and unexpectedly send out
The solubility property of existing particle is more preferable, can be with Flashmelt when bath is drunk.And the water of low temperature can be used (to be no more than 30
DEG C) dissolved, keep the activity of LBP-X not to be destroyed.
Further research is the immersion on matrimony vine in step 1).We are studied the soak to matrimony vine.
Scheme one, the matrimony vine in step 1) are soaked in water, and the temperature of water is 45 DEG C.
Scheme two, the matrimony vine in step 1) are soaked in ethanol, and the concentration of ethanol is 15%, and temperature is 40 DEG C.
Scheme three, the matrimony vine in step 1) are soaked in apple zymotic fluid, and temperature is 20 DEG C.
As a result find, for the blend-out of matrimony vine active composition and retain, it is excellent the depth of the night using scheme.Specifically, we also carry
The preparation method of described apple zymotic fluid is supplied：Using cider as raw material, pectase is added thereto, is liquefied；With de-
The de- hardship of bitter enzyme, add compound clarifier and stand clarification, the sugared ratio of acid is adjusted after deslagging；Advanced row alcoholic fermentation, then carry out acetic acid
Fermentation, then ageing at normal temperatures；The degerming and other impurity of freezing and filtering mode is finally used, that is, is obtained.More specifically, with
1000g ciders are raw material, add 3g pectases thereto, are liquefied；The de- hardship of bitter enzyme is taken off with 0.5g, stands, clarify, deslagging
Afterwards, adjustment acid sugar is than being 1:4；Advanced row alcoholic fermentation, then carry out acetic fermentation, then ageing at normal temperatures 12 hours；Finally
With the degerming and other impurity of freezing and filtering mode, that is, obtain.Soaked by the way of scheme three, greatly improve matrimony vine
Active material it is blend-out.
Beneficial effect：The granule being prepared using the method for the invention is the base in traditional decoction and syrup
The formulation developed on plinth, the advantages of decoction effect is rapid was both maintained, and overcome the trouble decocted temporarily again and easy mould evil idea goes bad
The shortcomings that.Meanwhile granule can dissolve or be suspended in water, is advantageous to medicine and absorbs in vivo, liquid preparation action is maintained
The characteristics of fast, but it is stable compared with liquid preparation property, it is easy to take, carries, stores.
Further, be not in that layering is present in preparation process using method of the present invention, mixed performance
Preferably.And dispersiveness, tack, aggregation, hygroscopicity are preferable, are advantageous to divided dose.
Further, using method of the present invention, the active component of matrimony vine is remained, greatly provides matrimony vine
Value.
Embodiment：
Embodiment 1 (soak is water)
Matrimony vine is soaked in 30min in 45 DEG C of water by step 1), is then beaten with beater, is obtained with filtered through gauze
Matrimony vine slurries；
Step 2) adds amylase in distilled water, and the addition of enzyme is the 0.5% of matrimony vine grind slurries quality.Between 30 DEG C
30min is activated, obtains enzyme mixation.
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
PH value is adjusted to 6.8.90 DEG C are progressively warming up to, enzyme deactivation 30min, is cooled to room temperature, is filtered, stands, takes supernatant, i.e., much
Sugar juice.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol (concentration 95%) precipitation.Distilled water washs repeatedly, dry Chinese holly
Qi polyoses extract.
The Lycium barbarum polysaccharide extract that step 5) obtains step, add maltodextrin, Icing Sugar, addition ethanol (concentration 80%)
For wetting agent softwood, then particle is made and crosses 12 mesh sieves, drying to obtain product.
Embodiment 2 (soak is water)
Matrimony vine is soaked in 35min in 45 DEG C of water by step 1), is then beaten with beater, is obtained with filtered through gauze
Matrimony vine slurries；
Step 2) adds amylase in distilled water, and the addition of enzyme is the 0.6% of matrimony vine grind slurries quality.Between 35 DEG C
35min is activated, obtains enzyme mixation.
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
PH value is adjusted to 6.8.90 DEG C are progressively warming up to, enzyme deactivation 35min, is cooled to room temperature, is filtered, stands, takes supernatant, i.e., much
Sugar juice.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol (concentration 95%) precipitation.Distilled water washs repeatedly, dry Chinese holly
Qi polyoses extract.
The Lycium barbarum polysaccharide extract that step 5) obtains step, add maltodextrin, Icing Sugar, addition ethanol (concentration 80%)
For wetting agent softwood, then particle is made and crosses 16 mesh sieves, drying to obtain product.
Embodiment 3 (soak is ethanol)
Matrimony vine is soaked in ethanol by step 1), and the concentration of ethanol is 15%, and temperature is 40 DEG C, 30min, then with mashing
Machine is beaten, and matrimony vine slurries are obtained with filtered through gauze；
Step 2) adds amylase in distilled water, and the addition of enzyme is the 0.5% of matrimony vine grind slurries quality.Between 30 DEG C
30min is activated, obtains enzyme mixation.
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
PH value is adjusted to 6.8.90 DEG C are progressively warming up to, enzyme deactivation 30min, is cooled to room temperature, is filtered, stands, takes supernatant, i.e., much
Sugar juice.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol (concentration 95%) precipitation.Distilled water washs repeatedly, dry Chinese holly
Qi polyoses extract.
The Lycium barbarum polysaccharide extract that step 5) obtains step, add maltodextrin, Icing Sugar, addition ethanol (concentration 80%)
For wetting agent softwood, then particle is made and crosses 12 mesh sieves, drying to obtain product.
Embodiment 4 (soak is ethanol)
Matrimony vine is soaked in ethanol by step 1), and the concentration of ethanol is 15%, and temperature is 40 DEG C, 35min, then with mashing
Machine is beaten, and matrimony vine slurries are obtained with filtered through gauze；
Step 2) adds amylase in distilled water, and the addition of enzyme is the 0.6% of matrimony vine grind slurries quality.Between 35 DEG C
35min is activated, obtains enzyme mixation.
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
PH value is adjusted to 6.8.90 DEG C are progressively warming up to, enzyme deactivation 35min, is cooled to room temperature, is filtered, stands, takes supernatant, i.e., much
Sugar juice.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol (concentration 95%) precipitation.Distilled water washs repeatedly, dry Chinese holly
Qi polyoses extract.
The Lycium barbarum polysaccharide extract that step 5) obtains step, add maltodextrin, Icing Sugar, addition ethanol (concentration 80%)
For wetting agent softwood, then particle is made and crosses 16 mesh sieves, drying to obtain product.
Embodiment 5 (prepares apple zymotic fluid)
Using 1000g ciders as raw material, 3g pectases are added thereto, are liquefied；The de- hardship of bitter enzyme is taken off with 0.5g, it is quiet
Put, clarify, after deslagging, adjusting acid sugar than being 1:4；Advanced row alcoholic fermentation, then acetic fermentation is carried out, then ageing at normal temperatures
12 hours；The degerming and other impurity of freezing and filtering mode is finally used, that is, is obtained.
Embodiment 6 (soak is apple zymotic fluid)
Matrimony vine is soaked in apple zymotic fluid by step 1), and temperature is 20 DEG C, 30min, is then beaten with beater,
Matrimony vine slurries are obtained with filtered through gauze；
Step 2) adds amylase in distilled water, and the addition of enzyme is the 0.5% of matrimony vine grind slurries quality.Between 30 DEG C
30min is activated, obtains enzyme mixation.
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
PH value is adjusted to 6.8.90 DEG C are progressively warming up to, enzyme deactivation 30min, is cooled to room temperature, is filtered, stands, takes supernatant, i.e., much
Sugar juice.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol (concentration 95%) precipitation.Distilled water washs repeatedly, dry Chinese holly
Qi polyoses extract.
The Lycium barbarum polysaccharide extract that step 5) obtains step, add maltodextrin, Icing Sugar, addition ethanol (concentration 80%)
For wetting agent softwood, then particle is made and crosses 12 mesh sieves, drying to obtain product.
Embodiment 7 (soak is apple zymotic fluid)
Matrimony vine is soaked in apple zymotic fluid by step 1), and temperature is 20 DEG C, 35min, is then beaten with beater,
Matrimony vine slurries are obtained with filtered through gauze；
Step 2) adds amylase in distilled water, and the addition of enzyme is the 0.6% of matrimony vine grind slurries quality.Between 35 DEG C
35min is activated, obtains enzyme mixation.
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value,
PH value is adjusted to 6.8.90 DEG C are progressively warming up to, enzyme deactivation 35min, is cooled to room temperature, is filtered, stands, takes supernatant, i.e., much
Sugar juice.
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol (concentration 95%) precipitation.Distilled water washs repeatedly, dry Chinese holly
Qi polyoses extract.
The Lycium barbarum polysaccharide extract that step 5) obtains step, add maltodextrin, Icing Sugar, addition ethanol (concentration 80%)
For wetting agent softwood, then particle is made and crosses 16 mesh sieves, drying to obtain product.
Embodiment 8 (determination of polysaccharide)
To embodiment 1~4, the Lycium barbarum polysaccharide extract obtained by the step 4 of embodiment 6~7 is detected, with different solvents
After the impurity such as monose, oligosaccharide, pigment in removal matrimony vine water extract, polyoses content is determined using phend-sulphuric acid, matrimony vine is more
The content of polysaccharide is as shown in the table in sugar extract.
| Polyoses content | |
| Embodiment 1 | 67.8% |
| Embodiment 2 | 68.6% |
| Embodiment 3 | 72.5% |
| Embodiment 4 | 74.9% |
| Embodiment 6 | 96.1% |
| Embodiment 7 | 89.2% |
Embodiment 9 (makes soft material to improve)
Experimental procedure is substantially the same manner as Example 6, and difference is, step 5 softwood processed is carried out in negative pressure, pressure
For -1mpa.
Embodiment 10 (makes soft material to improve)
Experimental procedure is substantially the same manner as Example 6, and difference is, step 5 softwood processed is carried out in negative pressure, pressure
For -0.5mpa.
Implement 11 (pelleting improves)
Experimental procedure is substantially the same manner as Example 6, and difference is, when particle is made in step 5, makes entirely to make pellet
Journey is carried out in the hot-air of flowing, and the temperature of hot-air is 35 DEG C, flow 0.8L/h.
Embodiment 12 (makes soft material, pelleting improves)
Experimental procedure is substantially the same manner as Example 6, and difference is, step 5 softwood processed is carried out in negative pressure, pressure
For -0.5mpa, when particle is made, whole pelleting process is set to be carried out in the hot-air of flowing, the temperature of hot-air is 35 DEG C,
Flow is 0.8L/h.
Embodiment 13 (granule detection)
By embodiment 6~7, the preparation-obtained LBP-X granule performance of embodiment 9~12 is carried out as follows
Detection：
The uniformity：Granule is taken to put the about 5cm that tiled in glossy paper in right amount2, its surface is flattened, observed at bright place, Ying Cheng
Now uniform color and luster, no decorative pattern and color spot.If with 10 times of lens examinations, there should not be the gloss (knot not crushed flashed
It is brilliant).If incomplete mixing, surface will have the different speckle of the depth.
Content uniformity inspection：Take granule 10 to wrap, weigh respectively.Often bag content weight should meet medicine compared with labelled amount
Regulation under allusion quotation content uniformity item.
The testing result of the LBP-X particle prepared by above-described embodiment is as shown in the table.
| The uniformity | Content uniformity | |
| Embodiment 6 | >96% | Meet regulation |
| Embodiment 7 | >95% | Meet regulation |
| Embodiment 9 | >98% | Meet regulation |
| Embodiment 10 | >98% | Meet regulation |
| Embodiment 11 | >98% | Meet regulation |
| Embodiment 12 | >99% | Meet regulation |
Embodiment 14 (dissolution velocity experiment)
By embodiment 6~7, the preparation-obtained LBP-X granule of embodiment 9~12 be dissolved in the experiment of warm water
(10g granules, being dissolved in 100ml water), test result is as follows
Embodiment 15 (the hypoglycemic experiment of granule drink)
Assay method reference：Shi Yutao etc. written " comparison of 2 kinds of Tea Polysaccharides blood sugar decreasing effects "《Hua Zhong Agriculture University
Journal》.By embodiment 1~4, embodiment 6~7, the preparation-obtained LBP-X granule of embodiment 9~12 is dissolved in warm water
Obtain drink and carry out hypoglycemic experiment, wherein model group is 15 through diabetic animal modeling, size of animal, and measurement result is such as
Under：
| Embodiment | Blood glucose value (%) (x ± s) |
| Embodiment 1 | 9.44±7.48 |
| Embodiment 2 | 9.90±7.88 |
| Embodiment 3 | 11.55±8.00 |
| Embodiment 4 | 10.01±6.98 |
| Embodiment 6 | 7.89±7.56 |
| Embodiment 7 | 7.99±6.99 |
| Embodiment 9 | 7.88±7.66 |
| Embodiment 10 | 7.95±6.77 |
| Embodiment 11 | 7.68±8.98 |
| Embodiment 12 | 7.40±9.22 |
| Blank group | 7.05±8.80 |
| Model group | 24.55±6.22 |
From experimental result as can be seen that this drink has hypoglycemic effect, made after being soaked in particular by apple zymotic fluid
The matrimony vine obtained expands Tang's granule drink, and it is more preferably notable by hypoglycemic effect, it may be possible to has certain synergy between component.
Claims (10)
1. a kind of preparation method of LBP-X particle, it is characterised in that carry out in accordance with the following steps：
Matrimony vine is soaked 30~35min by step 1), is then beaten with beater, matrimony vine slurries are obtained with filtered through gauze；
Step 2) adds enzyme in distilled water, and 30~35min is activated between 30~35 DEG C, obtains enzyme mixation；
Step 3) adds the matrimony vine slurries of gained in step 1 in step 2 in the enzyme mixation of gained, adjusts acid-base value, progressively
90 DEG C are warming up to, 30~35min of enzyme deactivation, is cooled to room temperature, is filtered, is stood, is taken supernatant, produce polysaccharide solution；
Step 4) and then it is concentrated under reduced pressure, adds absolute ethyl alcohol precipitation, distilled water washs repeatedly, dry Lycium barbarum polysaccharide extract；
The Lycium barbarum polysaccharide extract that step 5) obtains step, adds maltodextrin, Icing Sugar, and addition ethanol is that wetting agent system is soft
Material, then particle is made, cross 12~16 mesh sieves, drying to obtain product.
2. the preparation method of a kind of LBP-X particle according to claim 1, it is characterised in that described in step 2)
Enzyme is a kind of in amylase, cellulase；The addition of enzyme is the 0.5~0.6% of matrimony vine grind slurries quality.
A kind of 3. preparation method of LBP-X particle according to claim 1, it is characterised in that the regulation in step 3)
Acid-base value is that pH value is adjusted into 6.8.
A kind of 4. preparation method of LBP-X particle according to claim 1, it is characterised in that ethanol in step 4)
Concentration is 95%.
A kind of 5. preparation method of LBP-X particle according to claim 1, it is characterised in that ethanol in step 5)
Concentration is 80%；Raw material mass mixture ratio in step 5) is：2 parts of Lycium barbarum polysaccharide extract, 5~8 parts of dextrin, 5~8 parts of Icing Sugar.
A kind of 6. preparation method of LBP-X particle according to claim 1, it is characterised in that the softwood processed of step 5)
During carried out in negative pressure, pressure is -1~-0.5mpa.
A kind of 7. preparation method of LBP-X particle according to claim 1, it is characterised in that the matrimony vine in step 1)
It is soaked in water, the temperature of water is 45 DEG C.
A kind of 8. preparation method of LBP-X particle according to claim 1, it is characterised in that the matrimony vine in step 1)
It is soaked in ethanol, the concentration of ethanol is 15%, and temperature is 40 DEG C.
A kind of 9. preparation method of LBP-X particle according to claim 1, it is characterised in that the matrimony vine in step 1)
It is soaked in apple zymotic fluid, temperature is 20 DEG C.
A kind of 10. preparation method of LBP-X particle according to claim 9, it is characterised in that described apple fermentation
Liquid obtains by the following method：Using cider as raw material, pectase is added thereto, is liquefied；It is de- bitter with de- bitter enzyme, then add
Enter compound clarifier and stand clarification, the sugared ratio of acid is adjusted after deslagging；Advanced row alcoholic fermentation, then acetic fermentation is carried out, then normal
The lower ageing of temperature；The degerming and other impurity of freezing and filtering mode is finally used, that is, is obtained.
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| CN110326786A (en) * | 2019-07-29 | 2019-10-15 | 北京本草方源药业集团有限公司 | A kind of effective component of chinese medicine method for extracting high purity |
| CN110384237A (en) * | 2019-07-29 | 2019-10-29 | 北京本草方源药业集团有限公司 | A kind of single granule and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108617835A (en) * | 2018-05-04 | 2018-10-09 | 华东理工大学 | A kind of polysaccharides soft sweets and preparation method thereof |
| CN109897119A (en) * | 2019-03-07 | 2019-06-18 | 中国科学院过程工程研究所 | The method and purposes of pH value control and concentration in a kind of polysaccharides and polysaccharides preparation |
| CN110326786A (en) * | 2019-07-29 | 2019-10-15 | 北京本草方源药业集团有限公司 | A kind of effective component of chinese medicine method for extracting high purity |
| CN110384237A (en) * | 2019-07-29 | 2019-10-29 | 北京本草方源药业集团有限公司 | A kind of single granule and preparation method thereof |
| CN110384237B (en) * | 2019-07-29 | 2023-03-10 | 北京本草方源药业集团有限公司 | Single-ingredient granule and preparation method thereof |
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Application publication date: 20180116 |
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