CN112773823A - Preparation method of glabrous sarcandra herb extract and extract tablet - Google Patents
Preparation method of glabrous sarcandra herb extract and extract tablet Download PDFInfo
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- CN112773823A CN112773823A CN202110123213.3A CN202110123213A CN112773823A CN 112773823 A CN112773823 A CN 112773823A CN 202110123213 A CN202110123213 A CN 202110123213A CN 112773823 A CN112773823 A CN 112773823A
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- glabrous sarcandra
- sarcandra herb
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- 239000000594 mannitol Substances 0.000 description 1
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- LBDROUOCQSGOFI-UHFFFAOYSA-N methanol;phosphoric acid Chemical compound OC.OP(O)(O)=O LBDROUOCQSGOFI-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2013—Organic compounds, e.g. phospholipids, fats
- A61K9/2018—Sugars, or sugar alcohols, e.g. lactose, mannitol; Derivatives thereof, e.g. polysorbates
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2054—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/02—Drugs for skeletal disorders for joint disorders, e.g. arthritis, arthrosis
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- A—HUMAN NECESSITIES
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- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A61P7/00—Drugs for disorders of the blood or the extracellular fluid
- A61P7/04—Antihaemorrhagics; Procoagulants; Haemostatic agents; Antifibrinolytic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses a preparation method of glabrous sarcandra herb extract and extract tablets, which comprises the following steps: adding water into a container filled with the glabrous sarcandra herb raw material, and soaking for 20-50 minutes; (2) heating the container until the liquid medicine is boiled, decocting for 50-70 minutes, and filtering out the decoction; (3) adding water into the container for the second time, heating the container until the liquid medicine is boiled, decocting for 50-70 minutes, and filtering out the decoction; (4) adding water into the container for the third time, heating the container until the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out the decoction; (5) and combining the three decoctions, concentrating by using a triple-effect evaporation concentrator until the relative density is 1.26-1.30 at 75 ℃, and thus obtaining the glabrous sarcandra herb extract.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, and particularly relates to a glabrous sarcandra herb extract and a preparation method of glabrous sarcandra herb extract tablets.
Background
Herba Pileae Scriptae is dry whole herb of Sarcandra glabra (Thunb.) Nakai of Chloranthaceae. The chloranthaceae plant has 5 genera and about 70 more species all over the world, and is distributed in tropical zone or subtropical zone; the Chinese has 3 genera, about 18 species, is mainly distributed in places such as Sichuan, Yunnan, Guizhou, Anhui, Fujian, Jiangxi and the like, has wide distribution and rich resources, has long history of medicine taking, is bitter, pungent and mild in property, has the effects of clearing heat and cooling blood, activating blood and removing spots, dispelling wind and dredging collaterals, and is used for treating blood heat purpura, rheumatalgia and traumatic injury. In addition, modern researches show that the glabrous sarcandra herb has the effects of resisting tumors, resisting bacteria, diminishing inflammation, resisting platelet reduction and the like, is widely applied in the field of medicines and is collected in the section of pharmacopoeia of the people's republic of China 2015 edition. The glabrous sarcandra herb is widely distributed, has large resource storage amount, is easy to cultivate, has wide development prospect, and is widely applied to the fields of medicines, health products, foods, cosmetics, tobacco leaves and the like at present. The glabrous sarcandra herb tablet is a preparation produced by using glabrous sarcandra herb as a raw material, has the advantages of convenience in transportation, storage, taking and the like, and is a conventional preparation form.
However, the prior art glabrous sarcandra herb tablets have the defects of small preparation scale, low extraction and concentration efficiency and low content of effective components, so that new technology and method are needed to at least partially solve the problems in the prior art.
Disclosure of Invention
Therefore, the invention provides a preparation method of glabrous sarcandra herb tablets, which is characterized by comprising the following steps:
(1) adding water into the container filled with herba Pileae Scriptae raw material, soaking the medicinal materials in the water for 20-50 min until the water level is 30-50 cm;
(2) heating the container until the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out decoction;
(3) adding water into the container for the second time, wherein the water is 30-50cm above the surface of the medicine, heating the container until the medicine liquid is boiled, keeping the temperature of the medicine liquid at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out the decoction;
(4) adding water into the container for the third time until the water level is 30-50cm, heating the container until the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out the decoction;
(5) and combining the three decoctions, concentrating by using a triple-effect evaporation concentrator until the relative density is 1.26-1.30 at 75 ℃, and thus obtaining the glabrous sarcandra herb extract.
According to an embodiment of the invention, the operation of the triple effect evaporative concentrator comprises: the three-effect evaporation concentrator is in a negative pressure state by using a vacuum pump, the one-effect feed valve is opened for feeding, and the one-effect feed valve is closed when the combined decoction is fed to about 1/2 of the sight glass of the one-effect evaporation chamber; opening the double-effect feed valve for feeding, and closing the double-effect feed valve when the combined decoction is fed to about 1/2 of the double-effect evaporation chamber sight glass; the triple effect feed valve was then opened and closed when the combined simmer was fed to 1/2 of the triple effect evaporation chamber down-mirror.
According to an embodiment of the present invention, the operation of the triple effect evaporative concentrator further comprises concentrating after the feeding, wherein the concentrating comprises adjusting the vacuum control valve to make the primary vacuum at 0.03-0.05 Mpa, the evaporation temperature at about 90 ℃, the secondary vacuum at 0.05-0.07 Mpa, the evaporation temperature at about 75 ℃, the triple vacuum at 0.07-0.09 Mpa, and the evaporation temperature at about 55 ℃.
According to an embodiment of the present invention, it further comprises supplementing the combined decoctions during the concentration process.
According to another aspect of the present invention, there is provided a method for preparing glabrous sarcandra herb extract tablet, comprising drying and pulverizing glabrous sarcandra herb extract prepared according to the present invention, mixing with additives, and then granulating, press-forming to obtain glabrous sarcandra herb extract tablet.
According to an embodiment of the invention, the additive is selected from the group consisting of disintegrants, fillers, binders, lubricants and the like. For example, fillers may include starch, sugars, dextrin, lactose, compressible starch, microcrystalline cellulose, inorganic salts, mannitol, and the like; humectants and binders may include distilled water, ethanol, starch slurry, sodium carboxymethylcellulose, hydroxypropyl cellulose, methyl and ethyl cellulose, hydroxypropyl methyl cellulose, and the like; disintegrants may include dry starch, sodium carboxymethyl starch, low substituted hydroxypropyl cellulose, crospovidone, croscarmellose sodium, and the like; the lubricant may include magnesium stearate, silica gel micropowder, pulvis Talci, hydrogenated vegetable oil, polyethylene glycol, magnesium lauryl sulfate, etc.
Compared with the prior art, the method has the following advantages: can be used for large-scale industrial production. By adopting a specific extraction and concentration process, the efficiency can be improved, the content of effective components in the glabrous sarcandra herb extract and the glabrous sarcandra herb tablets can be increased, and a more beneficial treatment effect can be realized.
Detailed Description
The present invention is described in further detail below with reference to preferred embodiments, which are intended to be exemplary in nature and not to limit the application or uses of the disclosure.
The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples were purchased from a conventional reagent store unless otherwise specified.
Example 1
(1) Feeding: taking 200 kg/material and 3 kg/batch of glabrous sarcandra herb fragments, opening a feeding port, adding the glabrous sarcandra herb fragments into an extraction tank, and closing the feeding port.
(2) Adding water for the first time: adding water into the multifunctional extraction tank, observing water meter, closing the valve after the water level is 40cm above the medicine surface, and soaking for 30 min.
(3) Heating: and opening a steam valve, observing a pressure gauge, and heating to boil under the pressure of about 0.2 Mpa.
(4) First decoction: adjusting a steam valve after the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100 ℃, recording the decoction time of the liquid medicine, decocting for 1 hour, closing the steam valve, filtering the liquid medicine through a pipeline and a quick-opening filter, and storing the filtrate in a liquid storage tank.
(5) Adding water for the second time: adding water into the multifunctional extraction tank, observing water meter, and closing the valve after the water level is 40cm below the medicine surface.
(6) And (3) second decoction: and opening a steam valve, observing a pressure gauge, and heating to boil under the pressure of about 0.2 Mpa. Adjusting a steam valve after the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100 ℃, recording the decoction time of the liquid medicine, decocting for 1 hour, closing the steam valve, filtering the liquid medicine through a pipeline and a quick-opening filter, and storing the filtrate in a liquid storage tank.
(7) Adding water for the third time: adding water into the multifunctional extraction tank, observing water meter, and closing the valve after the water level is 40cm below the medicine surface.
(8) And (3) decocting for the third time: and opening a steam valve, observing a pressure gauge, and heating to boil under the pressure of about 0.2 Mpa. Adjusting a steam valve after the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100 ℃, recording the decoction time of the liquid medicine, decocting for 1 hour, closing the steam valve, filtering the liquid medicine through a pipeline and a quick-opening filter, and storing the filtrate in a liquid storage tank.
(9) And combining the three decoctions, transferring to a triple-effect evaporation concentrator, and concentrating.
(10) Starting a vacuum pump to enable the equipment to be at a negative pressure (-0.05 MPa or so), starting a discharge valve of the liquid medicine storage tank, starting a main feeding valve and an effective feeding valve to feed, and closing the effective feeding valve when the liquid medicine rises to 1/2 parts of a viewing mirror of an effective evaporation chamber. The two-effect feed valve is opened and closed when the feed liquid rises to 1/2 of the lower view mirror of the two-effect evaporation chamber. The three-effect feed valve is opened and closed when the feed liquid rises to 1/2 of the down-view mirror of the three-effect evaporation chamber.
(11) Then, concentration is carried out: adjusting a vacuum adjusting valve to ensure that the first-effect vacuum is at 0.04Mpa, the evaporation temperature is about 90 ℃, the second-effect vacuum is at 0.06Mpa, the evaporation temperature is about 75 ℃, the third-effect vacuum is at 0.08Mpa, and the evaporation temperature is about 55 ℃, so that the liquid material is concentrated in a concentrator, and when the temperature is too high, the steam inlet amount can be properly adjusted to be small.
(12) Replenishing liquid medicine: closing the steam valve, discharging vacuum, pumping the liquid medicine into the effective concentrator to the lower sight glass 1/2, closing the feed valve, closing the vacuum discharge valve, opening the steam valve, and continuing to concentrate to a small volume.
(13) When the liquid medicine is concentrated to a certain degree, the first-effect feeding valve is closed, the first-effect vacuum is kept, the second-effect and third-effect emptying valves are opened to break the vacuum, the second-effect and third-effect feeding valves are opened, the concentrated liquid of the second-effect and third-effect is pumped to the first-effect and is concentrated to the relative density of 1.26-1.30 (75 ℃).
And (3) process control: and when the concentrated solution is close to the preset requirement, the relative density of the liquid medicine is measured in time. During measurement, non-circulating feed liquid at a discharge port is discharged, and then the material is received and measured, and the material is qualified when the relative density is 1.26-1.30 (75 ℃), so that the glabrous sarcandra herb extract is obtained.
Example 2
(1) A high-temperature film is arranged on a clean stainless steel tray, a proper amount of starch (the starch is added in a weighing way and is recorded), 10kg of glabrous sarcandra herb extract obtained in the embodiment 1 is weighed, the glabrous sarcandra herb extract is spread on the starch, the thickness is about 1 cm, the tray is placed on a shelf, and the door of the cabinet is closed
(2) Starting a vacuum drying system, controlling the vacuum degree to be about 0.06MPa, starting a steam valve and an exhaust steam valve, controlling the temperature to be about 80 ℃, and drying for 24 hours to obtain dry paste;
(3) crushing the dry paste by a high-efficiency crusher;
(4) adding appropriate amount of adjuvants (starch), and mixing well by trough type mixer;
(5) granulating by a granulator, and pressing and forming to obtain the glabrous sarcandra herb extract tablet.
Experiment 1: detection of content of effective components in glabrous sarcandra herb extract
The content of three effective components of isofraxidin, rosmarinic acid and fumaric acid in the glabrous sarcandra herb extract is measured by an HPLC method.
Materials: glabrous sarcandra herb extract, mobile phase methanol-phosphoric acid and Agilent high pressure liquid chromatograph in example 1; an ultraviolet detector; an ultrasonic extractor and an ultrafine pulverizer.
The results show that: the mean content of the active ingredient isofraxidin in the glabrous sarcandra herb extract is 0.08%, the mean content of rosmarinic acid is 0.05%, and the mean content of fumaric acid is 0.10%, which is far higher than the content disclosed in the prior art.
Experiment 2: inhibition effect of oral glabrous sarcandra herb extract tablet on acute inflammation ear swelling of mice induced by dimethylbenzene
18 healthy mice were randomly divided into 3 groups, namely a model group, a positive control indomethacin group and a glabrous sarcandra herb extract tablet group. The method comprises the steps of performing normal saline intragastric administration (10ml/kg) on a model group, performing intragastric administration 0.01g/kg on an indomethacin group, performing intragastric administration 4g/kg on a glabrous sarcandra herb extract tablet group, continuously administering the medicine for 7 days, uniformly coating dimethylbenzene on the front and back surfaces of the right ear of a mouse of a positive control indomethacin group and the glabrous sarcandra herb extract tablet group after the medicine is administered on the 7 th day, performing postvertebralexanomyelia sacrifice for 4 hours to kill the mouse, cutting two ears along the base line of an auricle, respectively punching a round ear piece on the same position by using a puncher with the diameter of 8mm, weighing, and calculating swelling degree and inhibition rate of each group by taking the weight (mg) difference of the left ear piece. The average value of each mouse was determined and statistically processed, and the results are shown in table 1 below:
| group of | Dosage (mg/ml) | Right ear (mg) | Left ear (mg) | Degree of swelling |
| Model set | 18.37 | 14.12 | 4.26 | |
| Indomethacin | 1 | 17.03 | 14.85 | 2.18 |
| Glabrous sarcandra herb extract tablet | 400 | 17.34 | 15.13 | 2.21 |
The results show that: compared with a model group, the glabrous sarcandra herb extract tablet group has obvious difference (P is less than 0.01), has obvious effect of inhibiting acute inflammation and swelling of mouse ears caused by xylene, and has similar effect to that of an indomethacin group.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (6)
1. The preparation method of the glabrous sarcandra herb extract is characterized by comprising the following steps of:
(1) adding water into the container filled with herba Pileae Scriptae raw material, soaking the medicinal materials in the water for 20-50 min until the water level is 30-50 cm;
(2) heating the container until the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out decoction;
(3) adding water into the container for the second time, wherein the water is 30-50cm above the surface of the medicine, heating the container until the medicine liquid is boiled, keeping the temperature of the medicine liquid at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out the decoction;
(4) adding water into the container for the third time until the water level is 30-50cm, heating the container until the liquid medicine is boiled, keeping the temperature of the liquid medicine at 100-105 ℃, keeping the pressure in the container at 0.1-0.2Mpa, decocting for 50-70 minutes, and filtering out the decoction;
(5) and combining the three decoctions, concentrating by using a triple-effect evaporation concentrator until the relative density is 1.26-1.30 at 75 ℃, and thus obtaining the glabrous sarcandra herb extract.
2. The method of claim 1, wherein the operation of the triple-effect evaporative concentrator comprises: the three-effect evaporation concentrator is in a negative pressure state by using a vacuum pump, the one-effect feed valve is opened for feeding, and the one-effect feed valve is closed when the combined decoction is fed to about 1/2 of the sight glass of the one-effect evaporation chamber; opening the double-effect feed valve for feeding, and closing the double-effect feed valve when the combined decoction is fed to about 1/2 of the double-effect evaporation chamber sight glass; the triple effect feed valve was then opened and closed when the combined simmer was fed to 1/2 of the triple effect evaporation chamber down-mirror.
3. The method of claim 2, wherein the triple effect evaporation concentrator further comprises concentrating after the feeding, wherein the concentrating comprises adjusting the vacuum control valve to achieve a single effect vacuum of 0.03-0.05 Mpa, an evaporation temperature of about 90 ℃, a double effect vacuum of 0.05-0.07 Mpa, an evaporation temperature of about 75 ℃, a triple effect vacuum of 0.07-0.09 Mpa, and an evaporation temperature of about 55 ℃.
4. The method for preparing herba Pileae Scriptae extract of claim 3, further comprising supplementing the combined decoction during the concentration process.
5. A method for preparing a glabrous sarcandra herb extract tablet, which is characterized by comprising drying and crushing the glabrous sarcandra herb extract according to any one of claims 1 to 4, mixing the glabrous sarcandra herb extract with an additive, and then granulating and pressing to form the glabrous sarcandra herb extract tablet.
6. The method for preparing glabrous sarcandra herb extract tablet according to claim 5, wherein the additive is selected from the group consisting of a disintegrant, a filler, a binder and a lubricant.
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