CN114748512A - Method for rapidly extracting propolis - Google Patents
Method for rapidly extracting propolis Download PDFInfo
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- CN114748512A CN114748512A CN202210354507.1A CN202210354507A CN114748512A CN 114748512 A CN114748512 A CN 114748512A CN 202210354507 A CN202210354507 A CN 202210354507A CN 114748512 A CN114748512 A CN 114748512A
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- 241000241413 Propolis Species 0.000 title claims abstract description 94
- 229940069949 propolis Drugs 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 238000000605 extraction Methods 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 230000010355 oscillation Effects 0.000 claims abstract description 4
- 238000010298 pulverizing process Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 40
- 239000000126 substance Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 6
- 235000013871 bee wax Nutrition 0.000 claims description 3
- 239000012166 beeswax Substances 0.000 claims description 3
- 239000000110 cooling liquid Substances 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000005325 percolation Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000002137 ultrasound extraction Methods 0.000 description 7
- 229930003935 flavonoid Natural products 0.000 description 4
- -1 flavonoid compounds Chemical class 0.000 description 4
- 235000017173 flavonoids Nutrition 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000002481 ethanol extraction Methods 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000028327 secretion Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241001070941 Castanea Species 0.000 description 1
- 235000014036 Castanea Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000018522 Gastrointestinal disease Diseases 0.000 description 1
- 241000257303 Hymenoptera Species 0.000 description 1
- 206010020649 Hyperkeratosis Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/63—Arthropods
- A61K35/64—Insects, e.g. bees, wasps or fleas
- A61K35/644—Beeswax; Propolis; Royal jelly; Honey
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Insects & Arthropods (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Mechanical Engineering (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
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- Jellies, Jams, And Syrups (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a rapid extraction method of propolis, which relates to the field of propolis processing and comprises the following steps of S10, percolating and extracting the original propolis at room temperature, and storing primary percolate; step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of the filtrate, concentrating and drying to form purified propolis; step S30, freezing the purified propolis at low temperature, pulverizing and sieving; step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation. Purifying the original propolis by a percolation method to form purified propolis, then carrying out secondary extraction on the basis of the purified propolis, wherein impurities and interferents in the propolis extracted by the percolation method are fully removed, and the propolis can be fully dissolved after being dissolved in an alkaline ethanol solution, so that the extraction is finished; compared with the existing propolis extraction method, the extraction method has good effect and high efficiency.
Description
Technical Field
The invention relates to the field of propolis processing, in particular to a rapid extraction method of propolis.
Background
Propolis is a viscous substance formed by mixing secretions such as branches, leaf buds and callus of bees collected from plants, secretions such as jawbone and wax gland, and a small amount of pollen, is a very rare natural resource and is known as purple gold. In recent years, researches of scholars at home and abroad show that the propolis has important physiological effects of treating cardiovascular diseases, diabetes, skin diseases, gastrointestinal diseases, resisting cancers, enhancing immunity, resisting bacteria and diminishing inflammation and the like, is a hot spot in the field of health food research at present, has complex chemical components and contains phenol, acid, alcohol, ester, phenol, ether, alkene and various trace elements. The total flavone is one of the main active components of propolis for enhancing body immunity, softening blood vessel, reducing blood lipid and scavenging free radicals.
The modern propolis industrialized extraction method mainly comprises ethanol extraction and ultrasonic extraction, and most of components extracted by the two extraction methods are flavonoid compounds. The ultrasonic extraction mode is gradually reduced along with the equipment cost, is easier to scale and industrialize, and is gradually popularized.
However, in the existing ultrasonic extraction method, because the original propolis is not pretreated, the content of flavonoid compounds in the extract is low, the content of impurities similar to lead is high, and the extraction effect is poor.
Disclosure of Invention
In order to realize the purpose, the technical scheme adopted by the invention is as follows: a rapid extraction method of propolis comprises step S10, percolating and extracting raw propolis at room temperature, and storing primary percolate; step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of filtrate, concentrating and drying to form purified propolis; step S30, freezing the purified propolis at low temperature, pulverizing and sieving; step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation.
Further, step S30 is included after step S20, wherein the propolis ethanol solution is subjected to a filtration treatment to remove insoluble substances therein.
Further, in step S30, the propolis ethanol solution is filtered with a 200 mesh sieve.
Further, in step S30, the raw propolis is frozen in an environment of-20 to-40 degrees for 24 to 48 hours.
Further, in step S40, the method further includes step S41 of preparing an ethanol solution with a mass concentration ratio of 75% to 90%; step S42, heating the configured ethanol solution by using heating equipment, and keeping the constant temperature of 80 ℃; in step S43, a sodium hydroxide solution is added to the ethanol solution to adjust the pH of the ethanol solution to between 11 and 13.
Further, in step S40, when the original propolis piece is dissolved and ultrasonically vibrated, the original propolis piece is soaked in the ethanol solution for 15 to 20 minutes.
Further, in step S40, the frequency of the ultrasonic wave is between 25khz and 40khz, and the extraction time is 30 minutes.
Further, step S10 includes step S11 of percolating the vibrated mixed solution through a percolating device, and collecting a percolate; step S12, vacuum decompression concentration is carried out on the collected percolate, the extract is transferred into a settling tank, and stirring and cooling are carried out through stirring equipment; and step S13, standing and layering the cooling liquid, removing beeswax on the upper layer of the precipitation tank, concentrating the solution on the middle layer for later use, and discharging extract on the bottom layer to form purified propolis.
Further, step S13 is followed by step S14 of drying the extract at 105 degrees to constant weight by vacuum microwave drying.
Further, in step S13, the drying time was 30 minutes.
Compared with the prior art, the invention has the following beneficial effects:
firstly, purifying the original propolis by a percolation method to form purified propolis, then carrying out secondary extraction on the basis of the purified propolis, wherein impurities and interferents in the propolis extracted by the percolation method are fully removed, and the propolis can be fully dissolved after being dissolved in an alkaline ethanol solution, so that the extraction is finished; compared with the existing propolis extraction method, the extraction method has good effect and high efficiency.
Drawings
Fig. 1 is a schematic diagram of the working flow of propolis extraction in the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
Examples
As shown in fig. 1, the rapid extraction method of propolis in this embodiment includes the following steps,
step S10, percolating and extracting the original propolis at room temperature, and storing primary percolate;
step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of the filtrate, concentrating and drying to form purified propolis;
Step S30, freezing the purified propolis at low temperature, pulverizing and sieving;
step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation.
The modern propolis industrialized extraction method mainly comprises ethanol extraction and ultrasonic extraction, and most of components extracted by the two extraction methods are flavonoid compounds. The ultrasonic extraction mode is gradually reduced along with the equipment cost, is easier to scale and industrialize, and is gradually popularized.
However, in the existing ultrasonic extraction method, because the original propolis is not pretreated, the content of flavonoid compounds in the extract is low, the content of impurities similar to lead is high, and the extraction effect is poor.
In the scheme, the original propolis is purified by a percolation method to form purified propolis, and then secondary extraction is carried out on the basis of the purified propolis, because impurities and interferents in the propolis extracted by the percolation method are fully removed, the propolis can be fully dissolved after being dissolved in an alkaline ethanol solution, so that the extraction is finished; compared with the existing propolis extraction method, although the propolis extraction method is complex, the extraction effect is better and the efficiency is high.
Propolis is insoluble in water, slightly soluble in turpentine, partially soluble in ethanol, and soluble in 95% ethanol to give transparent chestnut color and granular precipitate. It is very soluble in ether, acetone and chloroform, and also in sodium hydroxide. Among the chemical substances, substances except ethanol are not common substances, and countries have strict regulations and limits on the application of the substances; the antibacterial property of propolis liquid extracted by ethanol is the strongest in all propolis extracting liquid at present. Thus, to date, ethanol has been the primary extraction solvent.
Referring to fig. 1, after step S20, step S30 is further included, wherein the propolis ethanol solution is subjected to a filtration treatment to remove insoluble substances therein;
particularly, can accomplish through centrifuge or the reciprocating sieve of aperture and filter, if the screen cloth that adopts in time filters, can select for use 200 meshes sieve, during the use, through getting rid of the insoluble substance in the propolis ethanol solution, firstly can prevent the pollution and the interference of insoluble substance to the propolis extract product, secondly also be convenient for retrieve the reuse to former propolis insoluble substance to avoid the waste on the material.
In step S30, the raw propolis is frozen in an environment of-20 to-40 degrees for 24h to 48h, preferably 36 h.
When in use, the original propolis can be quickly embrittled by cooling at low temperature, and the original propolis blocks can be frozen inside and outside after 36h of freezing.
Referring to fig. 1, in step S40, further includes the following,
step S41, preparing an ethanol solution with the mass concentration ratio of 75% to 90%; preferably, 75% ethanol is used as the extraction solvent of propolis;
step S42, heating the configured ethanol solution by using heating equipment, and keeping the constant temperature of 80 ℃; or carrying out water bath treatment at 80 ℃;
step S53, adding sodium hydroxide solution into the ethanol solution to adjust the pH value of the ethanol solution to between 11 and 13, preferably 12.5;
when the propolis tablet is used, the ethanol solution is adjusted to be alkaline and is subjected to constant-temperature water bath, and the organic extract in the original propolis block is more easily dissolved in the alkaline organic solution, so that the difficulty of subsequent extraction is reduced.
In step S40, when the original propolis block is subjected to ultrasonic wave vibration for dissolution, the original propolis block is soaked in an ethanol solution for 15 to 20 minutes; so as to dissolve the original propolis blocks as much as possible.
Furthermore, when the frequency of the ultrasonic wave is selected, the frequency can be selected from 25khz to 40khz, such as 25khz, 28khz and 40khz, and the ultrasonic wave is selected to vibrate the ethanol solution in which the original propolis blocks are dissolved, so that organic matters in the propolis can be crushed, and chemical bonds in the propolis can be broken to increase the dissolution of the propolis; further, the duration of ultrasonic extraction is about 30 minutes.
Referring to fig. 1, the following is included in step S10;
step S11, percolating and extracting the vibrated mixed solution through percolating equipment, and collecting percolate;
step S12, vacuum decompression concentration is carried out on the collected percolate, the extract is transferred into a settling tank, and stirring and cooling are carried out through stirring equipment;
and step S13, standing and layering the cooling liquid, removing beeswax on the upper layer of the precipitation tank, concentrating the solution on the middle layer for later use, and discharging extract on the bottom layer to form purified propolis.
After step S13, step S14 is included, wherein the extract is dried at 105 degrees by vacuum microwave drying to constant weight for approximately 30 minutes.
When the method is used, the primary extraction is carried out on the propolis by adopting a percolation method, and the purified propolis is primarily formed, so that impurities and insoluble substances in the propolis are reduced as much as possible during secondary purification, the purity of the propolis extract can be improved, and the difficulty of secondary purification can be reduced.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
The technical problems to be solved are still consistent with the present invention and should be included in the scope of the present invention.
Claims (10)
1. A rapid extraction method of propolis is characterized by comprising the following steps of S10, percolating and extracting raw propolis at room temperature, and storing primary percolate; step S20, stirring and cooling the primary percolate, standing for layering, taking a middle layer of filtrate, concentrating and drying to form purified propolis; step S30, freezing the purified propolis at low temperature, pulverizing and sieving; step S40, dissolving the purified propolis in ethanol solution, and extracting by ultrasonic oscillation.
2. The method as claimed in claim 1, further comprising a step S30 after the step S20, wherein the ethanol solution of propolis is filtered to remove insoluble substances.
3. The method for rapidly extracting propolis according to claim 2, wherein in step S30, the propolis ethanol solution is filtered by a 200-mesh sieve.
4. The method for rapidly extracting propolis according to claim 3, wherein in step S30, the raw propolis is frozen in an environment of-20 to-40 degrees for a period of time ranging from 24h to 48 h.
5. The method for rapidly extracting propolis according to claim 1, wherein in step S40, the method further comprises step S41 of preparing an ethanol solution with a mass concentration ratio of 75% to 90%; step S42, heating the configured ethanol solution by using heating equipment, and keeping the constant temperature of 80 ℃; in step S43, a sodium hydroxide solution is added to the ethanol solution to adjust the pH of the ethanol solution to between 11 and 13.
6. The method as claimed in claim 5, wherein the step S40 comprises immersing the propolis block in the ethanol solution for 15-20 minutes while subjecting the propolis block to ultrasonic wave for dissolution.
7. The method as claimed in claim 6, wherein in step S40, the frequency of the ultrasonic wave is between 25khz and 40khz, and the extraction time is 30 minutes.
8. The method for rapidly extracting propolis according to claim 1, wherein the step S10 includes a step S11 of percolating the mixed solution after shaking through a percolating device, and collecting a percolate; step S12, vacuum decompression concentration is carried out on the collected percolate, the extract is transferred into a settling tank, and stirring and cooling are carried out through stirring equipment; and step S13, standing and layering the cooling liquid, removing beeswax on the upper layer of the precipitation tank, concentrating the solution on the middle layer for later use, and discharging extract on the bottom layer to form purified propolis.
9. The method as claimed in claim 8, further comprising a step S14 after the step S13, drying the extract to constant weight at 105 degrees by vacuum microwave drying.
10. The method for rapidly extracting propolis according to claim 8, wherein in step S13, the drying time is 30 minutes.
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