CN104189517A - Ultramicro wall-broken gastrodia elata composition and preparation method thereof - Google Patents
Ultramicro wall-broken gastrodia elata composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of an ultramicro gastrodia elata decoction piece. The preparation method comprises selection of raw materials, cleaning of the raw materials, boiling, slicing, secondary boiling, drying, ultramicro wall breaking, obtaining of a preparation, and the like. Gastrodia elata processed by employing the processing and ultramicro fragmentation method has relatively high effective-composition dissolution rate, the bioavailability of a medicine is improved, the medicine effect is relatively good, and the toxicity is relatively low. The invention also discloses the decoction piece prepared by employing the method, and application of the decoction piece to prepare medicines for treating headache dizziness, numbness of limbs, infantile convulsion, epilepsy, twitch, tetanus and other diseases.
Description
Technical field
The application relates to a kind of preparation method of ultra micro Rhizoma Gastrodiae compositions, belongs to field of traditional Chinese.
Background technology
Rhizoma Gastrodiae (Gastrodia elata Bl.), claim again rhizoma gastrodiae, from mother, yellow moccasin flower, SHENCAO, solely shake sesame, rhizoma gastrodiae fat, DINGFENGCAO, close from grass, solely shake, automatically grass, water Rhizoma Solani tuber osi, RHIZONA GASTRODIAE etc., be the orchid family, Gastrodia herbaceos perennial, be distributed in national most areas.Its dry tuber also claims Rhizoma Gastrodiae, is to commonly use and famousr and precious Chinese medicine simply, the disease such as clinical dizzy, the numb limbs and tense tendons of being used for having a headache, infantile convulsion, epilepsy, tic, tetanus.
The conventional field of Chinese medicines, Rhizoma Gastrodiae generally adopts concocting method to process.The concocting method that < < Chinese Pharmacopoeia > > (2005 the 1st edition) records be " clean, run through or steam softly, shave, is dried ".But this concocting method has only been made regulation in principle, and does not point out concrete key parameter, thereby the Rhizoma Gastrodiae drug effect that adopts the distinct methods process of preparing Chinese medicine to obtain there are differences.
CN103285247A discloses a kind of preparation method of Processed Product of Rhizoma Gastrodiae, comprise selection, wash, dry, steaming and decocting, after drying, screening, packaging and other steps, the Processed Product of Rhizoma Gastrodiae that described method makes can not discharge the effective ingredient in Rhizoma Gastrodiae completely as far as possible, and gastrodin content is wherein relatively low.
Micro-powder of Chinese herbs is that a kind of of rising in recent years becomes micron and following powder body thereof with advanced physics or chemical means by Chinese drug preparation.The powder body of particle diameter 1～75 μ m is called " micropowder ", and the fine powder of particle diameter 0.1～1 μ m claims " superfine powder ".About the superfine powder of Chinese medicine, different researcheres has provided different titles and concept, as Chinese medicine ultramicro powder, single medicinal material ultramicro decoction piece, Chinese Traditional Medicine Powder etc.Somebody is that the micro-powder of Chinese herbs of object is called " cell grade micro-powder of Chinese herbs " by breaking cell.The feature of micro-powder of Chinese herbs is: Cellular Level Pulverizing, is conducive to drug-eluting; Increase drug absorption, improve bioavailability; Micronizing can be carried out under different temperatures, is conducive to retain active constituents of medicine, improves clinical efficacy; Take mouthfeel good, be convenient to application; Reduce dosage, reduce costs saving resource etc.Medical material is made after micropowder, can increase the stripping of effective ingredient, strengthens drug effect.But for the medicine containing toxic component, after micronizing, toxicity likely increases, and affects clinical drug safety.The median lethal dose(LD 50) (LD50) of the Semen Strychni common flour of the Study Mouses such as Jin Xinglin is 223.46mgkg
-1, the LD50 of Semen Strychni micropowder is 198.09mgkg
-1, this toxicity that shows Semen Strychni micropowder is greater than common flour, and showing has increased toxic component content after Semen Strychni micronization.
Summary of the invention
For the above-mentioned deficiency of prior art, the object of the present invention is to provide a kind of drug-eluting rate high, the ultra micro Processed Product of Rhizoma Gastrodiae that bioavailability is good and toxicity is low.
Above-mentioned purpose of the present invention is achieved by the following technical solution:
A preparation method for ultra micro Processed Product of Rhizoma Gastrodiae, comprises the steps:
2) will choose Rhizoma Gastrodiae and remove surperficial silt with high-pressure washing, then adopt the ultrasonic cleaning instrument degree of depth to clean; 3) Rhizoma Gastrodiae after cleaning is carried out to steaming and decocting under high pressure; 4) Rhizoma Gastrodiae after steaming and decocting under high pressure is cut into lamellar; 5) Rhizoma Gastrodiae section is soaked with Sucus Zingberis, then through steaming and decocting under high pressure; 6) by Rhizoma Gastrodiae chip drying, micronizing after secondary high-pressure steaming and decocting; 7) Rhizoma Gastrodiae ultra-micro powder is mixed with the excipient substance of micronizing, make ultra micro Processed Product of Rhizoma Gastrodiae.
Further, a kind of preparation method of ultra micro Processed Product of Rhizoma Gastrodiae, comprises the steps:
1) choose quality high-quality, full, without the Rhizoma Gastrodiae that goes mouldy, be raw material;
2) will choose Rhizoma Gastrodiae and remove surperficial silt with high-pressure washing, then adopt the ultrasonic cleaning instrument degree of depth to clean;
3) Rhizoma Gastrodiae after cleaning is carried out to steaming and decocting under high pressure;
4) Rhizoma Gastrodiae after steaming and decocting under high pressure is cut into lamellar;
5) Rhizoma Gastrodiae section is soaked with Sucus Zingberis, then through steaming and decocting under high pressure;
6) by Rhizoma Gastrodiae chip drying, micronizing after secondary high-pressure steaming and decocting;
7) Rhizoma Gastrodiae ultra-micro powder is mixed with the excipient substance of micronizing, make ultra micro Processed Product of Rhizoma Gastrodiae.
In the present invention, the size of the Rhizoma Gastrodiae stature in step 1 evenly.
In the present invention, the high-pressure washing that step 2 adopts can be under the pressure of 5-10MPa, repeatedly rinses 3-5 time, is preferably 3 times; The ultrasonic cleaning adopting preferably, at 30-80 ℃, is cleaned with the frequency of 40-80KHz, preferably, at 40 ℃, with the frequency of 40KHz, cleans, and the ultrasonic cleaning time is 10-50min, preferably 30min.
Adopt ultrasonic cleaning, can deep layer purify raw material, clean impurity.
In the present invention, the digestion time described in step 3 and 5 is controlled under the saturated vapor of 100-120 ℃, steaming and decocting 5-8 hour, preferably 6 hours.
In the present invention, the section described in step 4 can be carried out according to Rhizoma Gastrodiae size, and without strict dimensional requirement, generally speaking, for guaranteeing can more fully to mix with Sucus Zingberis before secondary boiled in step 5, slice size is controlled in the scope of 0.5-1cm.
In the present invention, step 5 adopts Sucus Zingberis to soak Rhizoma Gastrodiae section, wherein, and Rhizoma Gastrodiae: the weight ratio of Rhizoma Zingiberis Recens is 10:1-2.
In the preferred technical solution of the present invention, the preparation method of Sucus Zingberis: get Rhizoma Zingiberis Recens and smash extractive to pieces, filter, get filtrate, obtain.
In the preferred technical solution of the present invention, Sucus Zingberis soaks the preparation method of Rhizoma Gastrodiae section, soaks Rhizoma Gastrodiae section, soak time 3-5 hour, preferably 4 hours.
In the present invention, dry described in step 6 is selected from vacuum drying, drying under reduced pressure, spray-dired any or its combination.
In the preferred technical solution of the present invention, temperature is at 70-90 ℃, and be 10-15 hour drying time; Described micronizing is by being used for example mechanical impact crusher, jet mill, ball mill, vibromill or stirring mill to obtain.
In the preferred technical solution of the present invention, the particle diameter of Rhizoma Gastrodiae super-micro wall-broken powder, at 0.01-150 micron, is preferably 0.01-100 micron, most preferably is 0.1-50 micron.
In another embodiment, super-micro wall-broken Rhizoma Gastrodiae section of the present invention is decoction pieces type.Particularly, can make the decoction pieces type of all size, as: wafer thin: below 0.5mm; The circle of thin slice: 1～2mm, oblique, longitudinal and transverse; The circle of sheet: 2～4mm, oblique, longitudinal and transverse; Short section: 4～8mm; Stage casing: 8～12mm; Long section: 12～20mm; The square of piece sheet: 8～12mm and silk sheet: filament is that 2～3mm, crin are 5～10mm.
In the present invention, the pharmacy adjuvant described in step 7 is:
Filler, includes but not limited to lactose (crystallinity or powdery), dextrin, cane sugar powder, mannitol, glucose, sorbitol, fructose, erythrose, sodium chloride, starch (Semen Maydis, Rhizoma Solani tuber osi, Semen Tritici aestivi), microcrystalline Cellulose, dalcium biphosphate, magnesium carbonate, calcium carbonate, calcium sulfate, hydrolyzed starch, part alphalysed starch, synthetic aluminium silicate, special calcium silicates;
Adhesive, includes but not limited to methylcellulose, hydroxy methocel, hydroxypropyl emthylcellulose, sodium carboxymethyl cellulose, microcrystalline Cellulose, ethyl cellulose, Polyethylene Glycol, polyvinyl alcohol, polyvidone, sodium alginate, agar;
Disintegrating agent, includes but not limited to carboxymethyl starch sodium, cross-linking sodium carboxymethyl cellulose, polyvinylpolypyrrolidone, carboxymethyl cellulose, carboxymethylcellulose calcium, low-substituted hydroxypropyl cellulose, part alphalysed starch, microcrystalline Cellulose;
Lubricant, includes but not limited to magnesium stearate, calcium stearate, stearic acid, sodium lauryl sulphate, Stepanol MG, polyoxyethylene monostearate, Brij30;
Fluidizer, includes but not limited to Pulvis Talci, micropowder silica gel, wheaten starch.
In the present invention, because fiber content has certain influence to the mouthfeel of ultra-micro powder and result of use.As preferably, can to it, carry out solvent extraction alternatively according to fiber content in the Rhizoma Gastrodiae ultra-micro powder obtaining after micronizing.When fiber content too high, preferably in the step of the rear increase solvent extraction of step 6.Preferably, the solvent that this step adopts is water, extracts temperature and is controlled at below 60 ℃, for obtaining better extraction effect, preferably in leaching process, adopts sonic oscillation technology; The dry of extracting solution preferably adopts spraying dry.The Rhizoma Gastrodiae ultra-micro powder obtaining after dry carries out the preparation of step 7.
Preferably, above-mentioned solvent extraction step comprises following method:
A) Rhizoma Gastrodiae superfine powder is soaked to (for example, as 1-24 hour, 1-12 hour, 1-6 hour or 1-2 hour) through solvent as deionized water or ethanol water, extract being preferably no more than under the temperature conditions of 60 ℃;
B), by extracting liquid filtering, dry (preferably spray drying), obtains.The micronized pulverization step of step 6 a) is preferably carried out under the condition of sonic oscillation;
The concentration of the ethanol water step b) can be 1-90 % by weight, and for example 5-85 % by weight, 10-80 % by weight, as 20 % by weight, 30 % by weight, 40 % by weight, 50 % by weight or 60 % by weight etc.;
Described temperature can be for example 50 ℃, 40 ℃, 30 ℃ or 25 ℃.Step b) preferably include: extracting liquid filtering, filtrate are concentrated, (addition of oleic acid can be 0.1-0.8 times of Rhizoma Gastrodiae quality to add oleic acid, for example 0.2-0.5 doubly), use the shearing superfine grinding instrument of high speed centrifugation to pulverize, under vigorous stirring, add the doubly ethanol of (preferably 5-8 times, for example 6 or 7 times) of Rhizoma Gastrodiae quality 5-10, staticly settle, filter, dry, obtain.
In the present invention, by ultrasonic concussion, promote water or ethanol water collision even to penetrate crude drug cell wall, thereby fully extract the effective ingredient in medical material, and significantly improve extraction ratio, drug effect, drug quality and bioavailability thereof.
Another object of the present invention is to provide the Processed Product of Rhizoma Gastrodiae that a kind of said method prepares.
At above-mentioned decoction pieces of the present invention, comprise following component:
Preferably, the percentage by weight sum of above-mentioned each component is 100 weight portions.
In a specific embodiment, decoction pieces of the present invention comprises following component:
In the present invention, above-mentioned decoction pieces can be prepared as tablet, disintegrating agent, and the different dosage forms such as powder are preferably tablet.
Another object of the present invention is to provide a kind of above-mentioned decoction pieces and in preparation, treats the application in the medicine of the diseases such as headache is dizzy, numb limbs and tense tendons, infantile convulsion, epilepsy, tic, tetanus.
Compared with prior art, useful technique effect of the present invention is:
The dissolution rate of the Rhizoma Gastrodiae effective ingredient that the super-micro wall-broken treatment technology process of preparing Chinese medicine that the present invention adopts and the method for micronized pulverization are processed is higher, increased the bioavailability of medicine, and drug effect is better, and toxicity is lower.
The specific embodiment
Embodiment 1
10kg is best in quality, and the Rhizoma Gastrodiae that fresh nothing is gone mouldy, with 5MPa high pressure water washing three times, is removed silt, then at 40 ℃ with the ultrasonic cleaning 30min of 40KHz power; By after cleaning Rhizoma Gastrodiae as in high-pressure boiler, with 110 ℃ of vapour cookings 8 hours; Then the Rhizoma Gastrodiae obtaining is cut into the lamellar of 1cm; Separately get 1kg Rhizoma Zingiberis Recens, smash extractive to pieces, get Sucus Zingberis and soak Rhizoma Gastrodiae section 4 hours, and then as in pressure cooker with 120 ℃ of vapour cookings steaming and decocting in 8 hours; Then be placed in fallaway type baking oven at 75 ℃, dry 10 hours; Then adopt jet mill to carry out micronizing dry Rhizoma Gastrodiae section; By the Rhizoma Gastrodiae ultra-micro powder water supersound extract 2h at 60 ℃ obtaining, spraying is dry, finally Rhizoma Gastrodiae ultra-micro powder is mixed with starch, microcrystalline Cellulose, sodium lauryl sulphate and the magnesium stearate of micronizing, preparation, obtains ultra micro Processed Product of Rhizoma Gastrodiae.
Embodiment 2
15kg is best in quality, and the Rhizoma Gastrodiae that fresh nothing is gone mouldy, with 5MPa high pressure water washing three times, is removed silt, then at 40 ℃ with the ultrasonic cleaning 50min of 40KHz power; By after cleaning Rhizoma Gastrodiae as in high-pressure boiler, with 120 ℃ of vapour cookings 6 hours; Then the Rhizoma Gastrodiae obtaining is cut into the lamellar of 1cm; Separately get 3kg Rhizoma Zingiberis Recens, smash extractive to pieces, get Sucus Zingberis and soak Rhizoma Gastrodiae section 4 hours, and then as in pressure cooker with 120 ℃ of vapour cookings steaming and decocting in 8 hours; Then be placed in fallaway type baking oven at 85 ℃, dry 15 hours; Then adopt jet mill to carry out micronizing dry Rhizoma Gastrodiae section; Finally Rhizoma Gastrodiae ultra-micro powder is mixed with starch, microcrystalline Cellulose, sodium lauryl sulphate and the magnesium stearate of micronizing, preparation, obtains ultra micro Processed Product of Rhizoma Gastrodiae.
Embodiment 3
10kg is best in quality, and the Rhizoma Gastrodiae that fresh nothing is gone mouldy, with 5MPa high pressure water washing three times, is removed silt, then at 40 ℃ with the ultrasonic cleaning 30min of 40KHz power; By after cleaning Rhizoma Gastrodiae as in high-pressure boiler, with 120 ℃ of vapour cookings 8 hours; Then the Rhizoma Gastrodiae obtaining is cut into the lamellar of 1cm; Separately get 1kg Rhizoma Zingiberis Recens, smash extractive to pieces, get Sucus Zingberis and soak Rhizoma Gastrodiae section 5 hours, and then as in pressure cooker with 120 ℃ of vapour cookings steaming and decocting in 8 hours; Then be placed in fallaway type baking oven at 85 ℃, dry 15 hours; Then adopt jet mill to carry out micronizing dry Rhizoma Gastrodiae section; Finally Rhizoma Gastrodiae ultra-micro powder is mixed with starch, microcrystalline Cellulose, sodium lauryl sulphate and the magnesium stearate of micronizing, preparation, obtains ultra micro Processed Product of Rhizoma Gastrodiae.
Embodiment 4 gastrodin contents are measured
Adopt RP-HPLC method: chromatographic column Agilent Eclipse XDB-C18 (150mm * 4.6mm, 5 μ m); Mobile phase is acetonitrile-0.05% phosphate aqueous solution (3: 97); Flow velocity is 1.0mL/min; Column temperature is 25 ℃; Detection wavelength is 220nm.The gastrodine of the ultra micro Rhizoma Gastrodiae powder that embodiment 1-3 is made carries out assay.Results sample average recovery rate is 100.29%, RSD=1.82% (n=6).The gastrodin content of embodiment 1-3 is respectively 1.50%, 1.48% and 1.52%.
Claims (10)
1. a preparation method for ultra micro Processed Product of Rhizoma Gastrodiae, comprises the steps:
Optionally, 1) material choice: choose quality high-quality, full, without the Rhizoma Gastrodiae going mouldy, be raw material; With,
2) raw material cleans: the Rhizoma Gastrodiae that step 1 is obtained washes away Rhizoma Gastrodiae surface silt with water under high pressure, then adopts the ultrasonic cleaning instrument degree of depth to clean;
3) steaming and decocting: the Rhizoma Gastrodiae that step 2 is obtained is as for steaming and decocting in high-pressure boiler;
4) section: the Rhizoma Gastrodiae that step 3 is obtained is cut into lamellar;
5) secondary boiled: the Rhizoma Gastrodiae section that step 4 is obtained is soaked with Sucus Zingberis, and then as for steaming and decocting in pressure cooker;
6) dry: the Rhizoma Gastrodiae chip drying that step 5 is obtained;
7) super-micro wall-broken: micronizing is carried out in the Rhizoma Gastrodiae section that step 6 is obtained;
8) preparation: the Rhizoma Gastrodiae ultra-micro powder that step 7 is obtained mixes with the excipient substance of micronizing, preparation obtains ultra micro Processed Product of Rhizoma Gastrodiae.
2. method as claimed in claim 1, the high-pressure washing that step 2 adopts is under the pressure of 5-10MPa, repeatedly rinses 3-5 time, is preferably 3 times; The ultrasonic cleaning adopting is at 30-80 ℃, with the frequency of 40-80KHz, cleans, and preferably, at 40 ℃, with the frequency of 40KHz, cleans, and the ultrasonic cleaning time is 10-50min, preferably 30min.
Preferably, the digestion time described in step 3 and 5 is controlled under the saturated vapor of 100-120 ℃, steaming and decocting 5-8 hour, preferably 6 hours.
3. the method as described in claim 1-2 any one, the slice size described in step 4 is 0.5-1cm.
Preferably, described Rhizoma Gastrodiae section is decoction pieces type.Particularly, can make the decoction pieces type of all size, as: wafer thin: below 0.5mm; The circle of thin slice: 1～2mm, oblique, longitudinal and transverse; The circle of sheet: 2～4mm, oblique, longitudinal and transverse; Short section: 4～8mm; Stage casing: 8～12mm; Long section: 12～20mm; The square of piece sheet: 8～12mm and silk sheet: filament is that 2～3mm, crin are 5～10mm.
4. the method as described in claim 1-3 any one, step 5 adopts weight ratio Rhizoma Gastrodiae: the ratio that Rhizoma Zingiberis Recens is 10:1-2, get Rhizoma Zingiberis Recens and smash extractive to pieces, after filtration, to get Sucus Zingberis and soak Rhizoma Gastrodiae section, soak time was advisable with 3-5 hour, preferably 4 hours.
5. the method as described in claim 1-4 any one, employing vacuum drying oven or fallaway type oven drying that step 6 adopts, preferably fallaway type baking oven; Control temperature at 70-90 ℃, dry 10-15 hour; Described micronizing is to obtain by using mechanical impact crusher, jet mill, ball mill, vibromill or stirring mill; Ultra-micro powder particle diameter is in 0.01-150 micrometer range, and more preferably 0.01-100 micron, most preferably is 0.1-50 micron.
6. the method as described in claim 1-5 any one, is wherein also provided with the step that Ganoderma ultra-micro powder that step 6 is obtained carries out solvent extraction between step 6 and 7; Preferably under sonic oscillation, carry out, control temperature at 60 ℃, solvent is preferably water.
7. method as claimed in claim 6, is characterized in that, described solvent extraction step comprises following method:
A) Rhizoma Gastrodiae ultra-micro powder is soaked to (for example, as 1-24 hour, 1-12 hour, 1-6 hour or 1-2 hour) through solvent as deionized water or ethanol water, extract being preferably no more than under the temperature conditions of 60 ℃;
B), by extracting liquid filtering, dry (preferably spray drying), obtains;
Steps A) preferably under the condition of sonic oscillation, carry out; The concentration of the ethanol water steps A) can be 1-90 % by weight, preferably 5-85 % by weight, 10-80 % by weight, more preferably 20 % by weight, 30 % by weight, 40 % by weight, 50 % by weight or 60 % by weight; Described temperature is 50 ℃, 40 ℃, 30 ℃ or 25 ℃;
Step B) preferably include: extracting liquid filtering, filtrate are concentrated, (addition of oleic acid can be 0.1-0.8 times of Rhizoma Gastrodiae quality to add oleic acid, for example 0.2-0.5 doubly), use the shearing superfine grinding instrument of high speed centrifugation to pulverize, under vigorous stirring, add the doubly ethanol of (preferably 5-8 times, for example 6 or 7 times) of Rhizoma Gastrodiae quality 5-10, staticly settle, filter, dry, obtain.
8. the decoction pieces that prepared by the method as described in claim 1-7 any one, comprises following component:
The percentage by weight sum of above-mentioned each component is 100 weight portions.
9. decoction pieces as claimed in claim 8, comprises following component:
10. the decoction pieces that described in claim 1-7 any one prepared by method or the decoction pieces described in claim 8-9 are dizzy in preparation treatment headache, the application in the medicine of numb limbs and tense tendons, infantile convulsion, epilepsy, tic, tetanus disease.
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| CN105477059A (en) * | 2015-12-15 | 2016-04-13 | 安徽省康君食品有限公司 | Dehydrated salvia miltiorrhiza processing method |
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| CN109966257A (en) * | 2019-04-24 | 2019-07-05 | 安徽济顺中药饮片有限公司 | A kind of processing method of the prepared slices of Chinese crude drugs |
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Cited By (8)
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| CN105362720A (en) * | 2015-11-25 | 2016-03-02 | 苏州普罗达生物科技有限公司 | Ultra-micro wall-breaking pulverizing method for rhizoma gastrodiae |
| CN105477059A (en) * | 2015-12-15 | 2016-04-13 | 安徽省康君食品有限公司 | Dehydrated salvia miltiorrhiza processing method |
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| CN107802746A (en) * | 2017-11-13 | 2018-03-16 | 贵州景诚制药有限公司 | Rhizoma gastrodiae wall-broken decoction pieces and preparation method thereof |
| CN109430857A (en) * | 2018-10-23 | 2019-03-08 | 湖南舒元康健康科技有限公司 | A kind of food materials super-micro wall-broken processing method of integration of drinking and medicinal herbs |
| CN109966257A (en) * | 2019-04-24 | 2019-07-05 | 安徽济顺中药饮片有限公司 | A kind of processing method of the prepared slices of Chinese crude drugs |
| CN110123959A (en) * | 2019-06-24 | 2019-08-16 | 江西中医药大学 | A kind of preparation method of prepared Gastrodia medicine materical crude slice |
| CN112156154A (en) * | 2020-10-12 | 2021-01-01 | 华中农业大学 | Instant gastrodia tuber granules and preparation method thereof |
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