CN109646502A - One kind is rich in flavones Europe Lee fat capsule content and preparation method thereof - Google Patents
One kind is rich in flavones Europe Lee fat capsule content and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to Europe plum fruit deep process technology fields to provide a kind of rich in flavones Europe Lee fat capsule content and preparation method thereof to solve the problems, such as low, Europe Lee's oil in decreasing blood sugar effect difference of chromocor compound content etc. in current Europe Lee oil.It is prepared in proportion rich in flavones Europe Lee's fat capsule content by Europe Lee oil, Europe Lee's peel residue flavones extract, Euler's angle flavones extract, Europe Lee's organic acids extract, the vitamin E of fatty acids ethyl ester.Obtained Europe Lee's oil general flavone content is high, belong to endogenous flavones again, there are antioxidative synergistic effects with other active constituents such as organic acid, unsaturated fatty acid, Chinese medicine Europe Lee's feature is obvious, and Europe Lee oil activity is strong, can effectively improve reducing blood lipid and effect of weight reducing, process is easy to carry out, time saving, energy consumption is few, easy to industrialized production.
Description
Technical field
The invention belongs to Europe plum fruit deep process technology fields, and in particular to one kind is rich in flavones Europe Lee fat capsule content
Object and preparation method thereof.
Background technique
Europe Lee's oil is the extract of the kernel (also known as brush-cherry seed) for Chinese medicine Europe Lee.Europe Lee oil unsaturated lipid rich in
Fat acid, total amount only contain a small amount of saturated fatty acid up to 96 wt% or more.Main component is two kinds of fatty acid oleic acid (68.53%)
With linoleic acid (27.43%)；Oleic acid belongs to monounsaturated fatty acids (MUFA), has certain effect to blood lipid is reduced, occupies in Mediterranean
In the investigation of popular feelings blood vessel epidemiology, local resident's high fat diet is had found that while, but due to eating based on MUFA in diet
Olive oil (oleic acid content about 80%), cardiovascular morbidity is lower, and which results in experts to the weight of monounsaturated fatty acids
Depending on；Linoleic acid belongs to polyunsaturated fatty acid (PUFA), research shows that it is with stronger lipid-lowering effect.Euler's angle itself is
Integration of drinking and medicinal herbs Chinese medicine has stronger functions of loosening bowel relieving constipation containing active constituent amarogentin and flavonoids, can be to drop
Blood lipid plays synergistic effect.China's hyperlipemic patients and obesity continues to increase in recent years, the body for pursuing health become
These crowds there is an urgent need to.Market has had some grease type blood fat-reducing products such as fish oil, phosphatide, garlic oil etc. for treating
Disease is increased with prevention blood lipid, " controlling oil with oil " gets consumer reception very much, but lacks to extract using integration of drinking and medicinal herbs Chinese medicine as raw material and make
Standby grease type soft gel products.
Integration of drinking and medicinal herbs Chinese medicine has the characteristics that Product Safety is high, and soft capsule has convenient obvious advantage, from Europe
Li Ren extraction Europe Lee oil prepares soft capsule can meet the needs in market for hypolipemic function very well.Europe Lee's oil extract method has
Solvent method, squeezing method, supercritical CO2Extraction method etc., such as chromocor compound loss of Euler's angle functional component is more in extraction process,
In addition Euler's angle flavones source is single limited (kernel), Europe Lee's fat capsule content of preparation lacks flavones, it is difficult to reach drop
Blood lipid effect, it is therefore desirable to increase Europe Lee flavones content in Lee's fat capsule content of Europe to increase Europe Lee oil activity fat
Acid reduces blood lipid effect.Research is it has been shown that the antioxidant contents such as plant flavonoids ingredient, organic acid can make body from oxidation
Stress caused by metabolism disorder of blood lipid, and reduce blood lipid effective component.The plant flavones such as ginkgo, sea-buckthorn, hawthorn often by with
In hypolipemic function food.Europe Lee includes also containing a large amount of chromocor compounds in pericarp, pulp and kernel.Exploitation is rich in flavones
Europe Lee's fat capsule have very big market prospects.
Summary of the invention
The present invention is in order to solve asking for low, Europe Lee's oil in decreasing blood sugar effect difference of chromocor compound content etc. in current Europe Lee oil
Topic provides a kind of rich in flavones Europe Lee fat capsule content and preparation method thereof.
The present invention is realized by following technical solution: one kind being rich in flavones Europe Lee fat capsule content, by following weight
The raw material of part is prepared: 100 parts of Europe Lee oil of fatty acids ethyl ester, 5-10 parts of Europe Lee's peel residue chromocor extract, Euler's angle
1-3 parts of chromocor extract, 1-3 parts of Europe Lee's organic acids extract, 0.1-0.3 parts of vitamin E.
Preparation a kind of method rich in flavones Europe Lee's fat capsule content, it is characterised in that: steps are as follows:
(1) Euler's angle extracts: Euler's angle extracts to obtain Euler's angle oil and degreasing Euler's angle powder, Euler's angle using supercritical carbon dioxide
Ethyl alcohol is added in oil and lipase carries out ester exchange reaction, and after reaction, reactant is centrifuged 10 minutes for 3000 revs/min at room temperature,
Supernatant liquid oil is Europe Lee oil of fatty acids ethyl ester；50-75% ethanol water, Euler's angle are added in the Euler's angle powder of degreasing
The weight ratio of powder and ethanol water is 1:5；70-80 DEG C of heating and refluxing extraction 0.5-2h, filtering, 4 DEG C stand 24 hours, are precipitated
Filtering and removing slag after precipitating, to doing, 45 DEG C of vacuum drying 4h, the Euler's angle flavones for obtaining water content 4-10% mentions filtrate recycling design
Take object；
(2) preparation of Europe Lee peel residue chromocor extract, Europe Lee's organic acids extract: skin slag is added after taking the Europe 1000g Lee to squeeze the juice
The 60-95% ethanol water of 3-10 times of weight of skin slag, 70-80 DEG C is heated to reflux, and filters waste, collects filtrate, is concentrated, dry,
Get Ou Li peel residue chromocor extract；It takes 1000g cerasus humilis juice by anion-exchange column, after the completion of absorption, discards and pass through column
The fruit juice of son is collected whole organic acid portions with 5% aqueous hydrochloric acid solution elution anion-exchange column, is concentrated, dry, get Ou Li has
Machine acid extract；
(3) by fatty acids ethyl ester Europe Lee oil, Europe Lee's peel residue chromocor extract, Euler's angle chromocor extract, Europe Lee's organic acid
Heating stirring mixes in proportion for extract, vitamin E, centrifugation, and Europe Lee's fat capsule content of rich flavones is obtained after the de- ethyl alcohol of vacuum
Object.
The condition of supercritical carbon dioxide extraction Euler's angle are as follows: 30MPa, 45 DEG C.The addition of lipase in ester exchange reaction
Amount is the 1-10% of Euler's angle oil weight；The weight ratio of Euler's angle oil and ethyl alcohol is 1:0.01-0.15, and transesterification reaction temperature is
40-55 DEG C, ester exchange reaction time 0.5-3h.
Prepared organic acid optimal adsorption separation condition are as follows: anion-exchange column adsorbing separation temperature is 25-30 DEG C,
Applied sample amount is 1000g/100g resin, resin column bed height 400mm, adsorption flow rate 5-15ml/min, elution flow rate 2-3ml/
min。
Fatty-acid ethyl ester is content 1-10% in Europe Lee's fat capsule content mix object of prepared rich flavones；It is unsaturated
Content of fatty acid > 90%；General flavone content > 0.3%；Organic acid content is 0.10-0.80%.
Europe Lee's fat capsule content of prepared rich flavones carries out soft capsule packaging with the specification of 500-1000mg.
Euler's angle of the present invention extracts to obtain Euler's angle oil and degreasing Euler's angle powder using supercritical carbon dioxide, specifically extracts work
Skill is shown in document: application No. is ZL200410012382.6, entitled a kind of Europe Lee oil and preparation method thereof.
In Europe Lee's fat capsule content mix object of rich flavones prepared by the present invention general flavone from Europe plum fruit and
Kernel；Organic acid derives from Europe plum fruit；It include Europe Lee flavones, Ou Liyou in Europe Lee's fat capsule content mix object of rich flavones
The Multiple components such as machine acid, Europe Lee's oil ethyl ester, Europe Lee's oil unsaturated fatty acid are gained to be extracted using multiple means, then sufficiently mix
Conjunction obtains Euler's angle soft capsule content, and Chinese medicine Europe Lee's feature is obvious.Europe Lee's oil general flavone content that this method obtains is high, and belongs to
In endogenous flavones, there is antioxidative synergistic effects, Europe Lee oil activity with other active constituents such as organic acid, unsaturated fatty acid
By force, reducing blood lipid and effect of weight reducing can be effectively improved, process is easy to carry out, and time saving, energy consumption is few, easy to industrialized production.
Europe Lee's fat capsule content mix object of rich flavones prepared by the present invention is soft capsule content, is different from other
Suspension or dry-mixed dose.Since the ingredients such as Europe Lee's flavones are soluble in alcohol, it is insoluble in water and is also not readily dissolved in grease, if directly
It is mixed with grease, the cosolvent easy to form for mixing uneven body absorption difference or needing to add other auxiliary, the present invention
It solves the problems, such as that a large amount of flavones are dissolved in grease using containing contents ingredients such as fatty-acid ethyl ester Europe Lee's oil, therefore is not in inhale
Receive phenomenon difficult, that effect is poor.
Detailed description of the invention
Fig. 1 is Europe Lee's extract flavonoid components high-efficient liquid phase analysis result prepared by embodiment 1.
Specific embodiment
Embodiment 1: a kind of preparation method rich in flavones Europe Lee's fat capsule content includes the following steps:
(1) Euler's angle extracts: 4000g Euler's angle passes through supercritical CO2It extracts, extraction conditions: 30MPa, 45 DEG C, get Ou Li oil
1440g and degreasing Euler's angle 2115g；14.4g ethyl alcohol is separately added into this Europe Lee oil, immobilized lipase 14.4g, water 5g, instead
Temperature 45 C is answered, 0.5-3h is stirred, centrifugation goes enzyme to obtain fatty acids ethyl ester Europe Lee oil；Take 100g degreasing Euler's angle that weight is added again
70-80 DEG C of heating and refluxing extraction 0.5-2h of 50-75% ethanol water than 1:5 times is filtered, and stands 24 hours at 4 DEG C, is precipitated
Filtering and removing slag after precipitating, filtrate recycling design is to dry, then 45 DEG C of vacuum drying 4h, obtains water content 4-10% and obtains Euler's angle flavones
Extract, measurement general flavone content (colorimetric method, in terms of rutin, similarly hereinafter) are 0.77%.
(2) cerasus humilis juice extracts: taking 1000g cerasus humilis juice by 201 type of 100g anion-exchange column, (Tianjin Nankai is big
Learn chemical plant production), adsorbing separation temperature is 25-30 DEG C, 400 mm of resin column bed height, is adsorbed naturally, and coutroi velocity is
5-15ml/min after fruit juice liquid adsorbs, is eluted, elution flow rate 1- with twice of distilled water flushing pillar, then with 5% hydrochloric acid
Organic acid portion is collected in 3ml/min, pH test paper detection, is formed white precipitate with 1% silver nitrate solution and is detected that chloride ion occurs
When stop elution, collected organic acid soln is concentrated, is freeze-dried get Ou Li organic acid, organic acid content 25-41%(is neutralized
Titration, with citrometer, similarly hereinafter).The 60-95% ethyl alcohol heating of 3-10 times of weight ratio is added in skin slag after taking the Europe 1000g Lee to squeeze the juice
Filtrate is collected in reflux, filtering, and concentration stands slagging-off, and clear liquid is freeze-dried to obtain Europe plum fruit chromocor extract, colorimetrically analysing
General flavone content is 6.25%.Liquid chromatographic detection contains rutin 0.92mg/ml, Quercetin 0.51mg/ml and Kaempferol flavones
0.05mg/ml ingredient (see attached drawing 1)；
(3) by fatty acids ethyl ester Europe Lee oil 500g, Europe Lee peel residue chromocor extract 30g, Euler's angle chromocor extract 5g, Europe
5g parts of Lee's organic acids extract, vitamin E 0.5g, heating stirring, mixes in proportion, filtering, obtains after the de- ethyl alcohol of filter vacuum rich
Europe Lee's fat capsule content mix object of flavones.General flavone content 335mg/100g(colorimetric method in mixture)；Gas-chromatography point
Condensate oil rouge unsaturated fatty acid 95.1%, fatty-acid ethyl ester content 4.5%, organic acid content 0.10%.
(4) mixture is subjected to soft capsule packaging with the specification of 1000mg.
Embodiment 2: a kind of preparation method rich in flavones Europe Lee's fat capsule content, according to side described in embodiment 1
Method prepares fatty acids ethyl ester Europe Lee oil, Europe Lee's peel residue chromocor extract, Euler's angle chromocor extract, Europe Lee's organic acid extract
Object.
(1) by fatty acids ethyl ester Europe Lee oil 500g, Europe Lee peel residue chromocor extract 50g, Euler's angle chromocor extract
10g, Europe Lee organic acids extract 10g, vitamin e1 .0g, heating stirring, mixes in proportion, filtering, after filter vacuum takes off ethyl alcohol
Obtain Europe Lee's fat capsule content mix object of rich flavones.Colorimetric method (in terms of rutin) general flavone content 550mg/ in mixture
100g；Gas chromatography analysis unsaturated fatty acid 95.1%, fatty-acid ethyl ester content 9.5%, organic acid content 0.25%.
(2) mixture is subjected to soft capsule packaging with the specification of 1000mg.
Embodiment 3: one kind being rich in flavones Europe Lee's fat capsule, includes the following steps: fatty according to preparing in embodiment 1
Acetoacetic ester Europe Lee oil, Europe Lee's peel residue chromocor extract, Euler's angle chromocor extract, Europe Lee's organic acids extract.
(1) by fatty acids ethyl ester Europe Lee oil 500g, Europe Lee peel residue chromocor extract 25g, Euler's angle chromocor extract
15g, Europe Lee organic acids extract 15g, vitamin e1 .5g, heating stirring, mixes in proportion, filtering, after filter vacuum takes off ethyl alcohol
Obtain Europe Lee's fat capsule content mix object of rich flavones.In mixture (in terms of rutin) general flavone content 310mg/100g；Gas phase
Chromatography analysis unsaturated fatty acid 96.1%, fatty-acid ethyl ester content 1.0%, organic acid content 0.80%.
(2) mixture is subjected to soft capsule packaging with the specification of 500mg.
Embodiment 4: means of supercritical extraction Europe Lee's oil 500g does not add other extracts in Example 1, and colorimetric method is (with rutin
Meter) measurement general flavone content be 35mg/100g；Gas chromatography analysis fatty-acid ethyl ester 0%, unsaturated fatty acid 94.5%, has
Machine acid content 0.02%.Europe Lee's oil is subjected to soft capsule packaging with the specification of 500mg.
Embodiment 5:DPPH1,1- diphenyl -2- trinitrophenyl-hydrazine radicals scavenging experiment: pipette extraction embodiment is used
Europe Lee's oil obtained by 1-4 is configured to Europe Lee's oil solution that concentration is 0.5mg/ml using 95% ethyl alcohol；This solution of 1.5ml is drawn to add
Enter in 10ml centrifuge tube, add the DPPH solution of the 0.025mg/ml of equivalent, judder is placed on dark place, at room temperature instead
30 min are answered, its absorbance (A1) at 517nm, same method detection 1.5ml DPPH solution and 1.5ml are detected
Absorbance (the A of 95% ethyl alcohol0) and the Europe 1.5ml Lee's oil solution and 95% ethyl alcohol of 1.5ml absorbance (A2).
DPPH free radical scavenging activity (%)=[1- (A1-A2)/A0]*100
Europe Lee's oil obtained by 1 embodiment 1-4 of table carries out external removing free radical
Seen from table 1, the embodiment 1-3 free radical scavenging activity (75.5%, 85.3% and 75.0%) rich in flavones is greater than compared with embodiment
4 free radical scavenging activities (58.1%) show that Europe Lee's oil has stronger radicals scavenging effect.
Embodiment 6: charcoal end propulsion functions experiment
Proper amount of active carbon is added to be configured to aqueous suspension Europe Lee's oil obtained by embodiment 1-4, wherein 0.05g/ml containing active carbon, crude drug
Measure 1g/ml.
Small white mouse similar in 24 hours weight of fasting is taken out, by its random grouping, is divided into 4 groups, every group 6, uses marking pen
It marks, then respectively with different charcoal end liquid 0.2ml/10g weight stomach-fillings, control group is mixed to isometric physiological saline charcoal end
Suspension, cervical vertebra is put to death after twenty minutes for administration, is cut open the belly immediately, is opened abdominal cavity and is separated mesenterium, is cut off upper end and is extremely returned from pylorus, lower end
The intestinal tube in blind portion is used as " total small intestinal length ", and the distance using pylorus to charcoal end forward position is counted as " charcoal end in the intestine advance distance "
Calculate the percentage that charcoal end advance distance accounts for small intestine overall length, value X ± s(mean ± standard deviation) it indicates.Charcoal is calculated with formula
Last ink propulsive rate:；
Europe Lee's oil obtained by 2 embodiment 1-4 of table carries out external removing free radical
As can be seen from Table 2, Europe Lee's oil obtained by embodiment 1-3 has preferable charcoal end propulsion functions, Europe Lee more lower than flavones content
Oil display has stronger enterocinesia effect, it may be possible to which Europe Lee's flavones is related with effect under the letting out of Europe Lee's oil.
Embodiment 7: rat lipid-lowering test: Europe Lee's oil obtained by embodiment 1-4 is subjected to hyperlipidemia model rat oral gavage and drops blood
Rouge, high in fat group of feeding high lipid food, normal group feeding arm's length basis feed.Female wistar rat (42): high lipid food (from
System): 78.8% basal feed；1% cholesterol；0.2% bovine bile；10% yolk powder；10% lard.Basal feed (self-control): 73.5%
Corn flour;20% wheat bran；5% fish meal；1% flour；0.5% salt.
Experimental group embodiment 1-4 group, model group and totally 6 groups of blank group, every group of 6 rats feed basis before experiment
Feed and free water, which are observed, to be adapted to 3 weeks.When experiment, embodiment 1-4 group feeds high lipid food 15g/d Jia Ouli oil 1.5ml/d；Mould
Type group group high lipid food 15g/d adds physiological saline 1.5ml/d, and the normal basal feed 15g/d that organizes adds physiological saline 1.5ml/d, even
It is 40 days continuous；Experiment terminates, rat anesthesia, and abdominal aorta blood sampling measures blood lipid indices after separating serum.
Influence of the Europe Lee's oil to hyperlipemia rat reducing blood lipid index obtained by 3 embodiment 1-4 of table
Note: letter a indicates that significant difference (P < 0. 05) compared with the control group, b indicate extremely significant (the P < of difference in table
0.01)；C indicates that the significant difference (P < 0. 05) compared with normal group, d indicate that difference is extremely significant (P < 0.01).
Seen from table 3, Europe Lee's oil serum TG difference compared with model group rich in flavones is not significant for embodiment 4.And it is real
It is all low compared with model control group level to apply a 1-3 serum TG, and difference is all significant, embodiment 2 is even up to extremely significant；Serum TC
Content is lower compared with model group, significant difference.Embodiment 1-3 high-density lipoprotein cholesterol (HDL-C) is increased compared with model group,
Its level is compared with compareing blank group, close to the blank group of basal feed, shows that the effect of its reducing blood lipid close to normal level, is shown
Work property test significant difference, shows that Europe Lee's oil rich in flavones has stronger effect for reducing blood fat.
Embodiment 8: to 1 Europe Lee's extract flavonoid components high-efficient liquid phase analysis of embodiment.See Fig. 1；It can be obtained according to Fig. 1,
Ou Lizhong contains rutin, Quercetin, Kaempferol, respectively chromatographic peak 1, chromatographic peak 2, chromatographic peak 3, calculates rutin in Europe Lee oil
0.92mg/ml, Quercetin 0.51mg/ml and Kaempferol flavones 0.05mg/ml ingredient.
Europe Lee's fat capsule content mix object of rich flavones prepared by the present invention is soft capsule content, is different from other
Suspension or dry-mixed dose.Since the ingredients such as Europe Lee's flavones are soluble in alcohol, it is insoluble in water and is also not readily dissolved in grease, if directly
It is mixed with grease, the cosolvent easy to form for mixing uneven body absorption difference or needing to add other auxiliary.The present invention utilizes
It solves the problems, such as that a large amount of flavones are dissolved in grease containing contents ingredients such as fatty-acid ethyl ester Europe Lee's oil, therefore is not in absorb to be stranded
Phenomenon difficult, effect is poor.
Claims (7)
1. one kind is rich in flavones Europe Lee fat capsule content, it is characterised in that: be prepared: being contained by the raw material of following parts by weight
100 parts of Europe Lee oil of fatty-acid ethyl ester, 5-10 parts of Europe Lee's peel residue chromocor extract, 1-3 parts of Euler's angle chromocor extract, Ou Li
1-3 parts of organic acids extract, 0.1-0.3 parts of vitamin E.
2. preparing a kind of method rich in flavones Europe Lee's fat capsule content described in claim 1, it is characterised in that: step
It is as follows:
(1) Euler's angle extracts: Euler's angle extracts to obtain Euler's angle oil and degreasing Euler's angle powder, Euler's angle using supercritical carbon dioxide
Ethyl alcohol is added in oil and lipase carries out ester exchange reaction, and after reaction, reactant is centrifuged 10 minutes for 3000 revs/min at room temperature,
Supernatant liquid oil is Europe Lee oil of fatty acids ethyl ester；50-75% ethanol water, Euler's angle are added in the Euler's angle powder of degreasing
The weight ratio of powder and ethanol water is 1:5；70-80 DEG C of heating and refluxing extraction 0.5-2h, filtering, 4 DEG C stand 24 hours, are precipitated
Filtering and removing slag after precipitating, to doing, 45 DEG C of vacuum drying 4h, the Euler's angle flavones for obtaining water content 4-10% mentions filtrate recycling design
Take object；
(2) preparation of Europe Lee peel residue chromocor extract, Europe Lee's organic acids extract: skin slag is added after taking the Europe 1000g Lee to squeeze the juice
The 60-95% ethanol water of 3-10 times of weight of skin slag, 70-80 DEG C is heated to reflux, and filters waste, collects filtrate, is concentrated, dry,
Get Ou Li peel residue chromocor extract；It takes 1000g cerasus humilis juice by anion-exchange column, after the completion of absorption, discards and pass through column
The fruit juice of son is collected whole organic acid portions with 5% aqueous hydrochloric acid solution elution anion-exchange column, is concentrated, dry, get Ou Li has
Machine acid extract；
(3) by fatty acids ethyl ester Europe Lee oil, Europe Lee's peel residue chromocor extract, Euler's angle chromocor extract, Europe Lee's organic acid
Heating stirring mixes in proportion for extract, vitamin E, centrifugation, and Europe Lee's fat capsule content of rich flavones is obtained after the de- ethyl alcohol of vacuum
Object.
3. the method that preparation according to claim 2 is rich in flavones Europe Lee fat capsule content, it is characterised in that: super to face
The condition of boundary's carbon dioxide draw Euler's angle are as follows: 30MPa, 45 DEG C.
4. the method that preparation according to claim 2 is rich in flavones Europe Lee fat capsule content, it is characterised in that: organic
Sour absorption separation condition are as follows: anion-exchange column adsorbing separation temperature is 25-30 DEG C, and applied sample amount is 1000g/100g resin, tree
Rouge column bed height 400mm, adsorption flow rate 5-15ml/min, elution flow rate 2-3ml/min.
5. the method that preparation according to claim 2 is rich in flavones Europe Lee fat capsule content, it is characterised in that: ester is handed over
The additional amount for changing lipase in reaction is the 1-10% of Euler's angle oil weight；The weight ratio of Euler's angle oil and ethyl alcohol is 1:0.01-
0.15, transesterification reaction temperature is 40-55 DEG C, ester exchange reaction time 0.5-3h.
6. the method that preparation according to claim 2 is rich in flavones Europe Lee fat capsule content, it is characterised in that: made
Fatty-acid ethyl ester is content 1-10% in Europe Lee's fat capsule content mix object of standby rich flavones；Unsaturated fatty acid content >
90%；General flavone content > 0.3%；Organic acid content is 0.10-0.80%.
7. according to claim 1 a kind of rich in flavones Europe Lee fat capsule content, it is characterised in that: described rich in Huang
Ketone Europe Lee's fat capsule content carries out soft capsule packaging with the specification of 500-1000mg.
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