CN109125258A - A kind of preparation method of intensified loquet distillate - Google Patents

A kind of preparation method of intensified loquet distillate Download PDF

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Publication number
CN109125258A
CN109125258A CN201811252712.7A CN201811252712A CN109125258A CN 109125258 A CN109125258 A CN 109125258A CN 201811252712 A CN201811252712 A CN 201811252712A CN 109125258 A CN109125258 A CN 109125258A
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preparation
intensified loquet
loquet distillate
enriched
sucrose
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CN109125258B (en
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徐玉琴
梅璇
潘忠平
王志敏
叶帮伟
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China Resources Sanjiu Nanchang Pharmaceutical Co Ltd
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China Resources Sanjiu Nanchang Pharmaceutical Co Ltd
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Abstract

The present invention provides a kind of preparation methods of intensified loquet distillate, in being formulated in addition to menthol, the Six-elements such as remaining loguat leaf add water to cook secondary, 2 hours every time, collecting decoction, filtration, concentration, it is centrifuged again, centrifugate decocts, and it is enriched with after concentration, improve intensified loquet distillate effective component integrally, sediment in technique traditional Chinese medicine extraction of the invention is removed to 5/10000ths or more, the clarity of product is effectively ensured, it improves existing intensified loquet distillate product and easily occurs the quality precipitated on a small quantity in storage, the risk that microorganism occurs in product simultaneously substantially reduces, mouthfeel is more preferable.

Description

A kind of preparation method of intensified loquet distillate
Technical field
The invention belongs to field of traditional Chinese medicine pharmacy, and in particular to a kind of preparation method of intensified loquet distillate.
Background technique
Intensified loquet distillate is light brown supernatant liquid；Gas is fragrant, sweet.Yin-nourishing astringing lung-QI, cough-relieving apophlegmatic.For bronchitis cough It coughs.Main component is loguat leaf, pappy shell, the tuber of stemona, Cynanchum glaucescens, the root bark of white mulberry, campanulaceae, menthol.Loguat leaf, root bark of white mulberry clearing lung-heat, hundred Lung drops in portion's moistening lung, pappy shell astringing lung-QI, campanulaceae promoting the dispersing function of the lung, Cynanchum glaucescens.Major function: yin-nourishing astringing lung-QI, kobadrin.For chronic cough due to asthenia of viscera, Bronchitis etc..
The prior art such as " intensified loquet distillate and preparation method thereof " CN200510010324.4, the present invention relates to a kind of strengths Loquat dew and preparation method thereof, seven taste such as loguat leaf, in addition to menthol, the Six-elements Chinese medicine such as remaining loguat leaf add water to cook it is secondary, 2 hours every time, collecting decoction, filtration was concentrated into relative density of medicine liquid 1.13-1.15, and Steviosin 2g is added to dissolve, and citron is added Sour 0.5g is stirred, is mixed, stood with ethyl alcohol dissolution essence is appropriate and menthol, and filtration adds water to 1000ml, mix to get. For another example: " intensified loquet distillate and preparation method thereof " CN201110111681.5, the weight ratio g of intensified loquet distillate of the invention are as follows: Loguat leaf 50g, pappy shell 45g, tuber of stemona 10g, Cynanchum glaucescens 6g root bark of white mulberry 4g, campanulaceae 4g, menthol 0.09g；Preparation method be except Outside menthol, the Six-elements such as remaining loguat leaf add water to cook it is secondary, 2.5 hours every time, collecting decoction, filtration, be concentrated into 700ml, Add sodium benzoate 2.6g, stirring adds sucrose 700g, continue to be heated to boiling to dissolving, and keeps the temperature 30 minutes, stands, and filtration adds water To 1200ml, mix to get.Substantially by secondary decoction, filtering, concentration is made this technology, but facts have proved according to said method Intensified loquet distillate obtained finds that will appear a little atrament after being long placed in precipitates during storage, and vulnerable to high temperature illumination It influences, to increase microbiological hazards, even results in the bottle that rises, there is high risk, and bitter taste can not be made to be reduced to satisfaction The agreeable to the taste requirement of user, and due to the main ingredient that loguat leaf is intensified loquet distillate, because each place of production loquat leaf composition has slightly not Together, according to loguat leaf modern industry planting requirement and loquat growth characteristics, under a large amount of trimmings that planting loquat process is generated Come or the loguat leaf that withers and falls naturally is as raw material, the trend that the effective component that loguat leaf has stored long is reduced, in addition Pi Have the tendency that variety deterioration in rake leaf planting process, causes the active constituent content in loguat leaf to be declined, by traditional handicraft There are content deficiencies for the effective component of extraction, it is possible to need enrichment method or broken wall pre-treatment that active principle is made to reach suitable Content, such as Corosolic acid, euscaphic acid triterpene sour component belong to effective component.Therefore how to effectively improve clarity, mention High main ingredient active principle content and reduction microbiological hazards are showed no all in patent disclosed so far and non-patent literature There is referential technical inspiration, the technical solution that lower but face will be introduced generates in this background.
Summary of the invention
Not high for traditional handicraft loguat leaf effective component extraction rate, strength loquat reveals the existing precipitating risk of product and micro- Biological risk, by study increase in production technology decocted again after centrifugation, centrifugation after concentrate is decocted, decocted etc. processes or Enrichment and loguat leaf broken wall pre-treating technology, efficiently solve the problems, such as this from technique after concentration.
The object of the present invention is to provide a kind of preparation method of intensified loquet distillate, increase centrifugation, centrifugate decoct step with Precipitating and microbiological hazards are reduced, it is a further object of the present invention to provide a kind of main ingredient loguat leaf pre-treating methods, make loguat leaf Extraction is more complete, provides a kind of concentrate enrichment method, and making intensified loquet distillate integrally is that active principle content increases, particular for Triterpenic acid effective component is enriched in loguat leaf.
The purpose of the present invention is what is implemented by following technical proposal:
A kind of preparation method of intensified loquet distillate, every 1000ml intensified loquet distillate are prepared by following raw material and parts by weight: Loguat leaf 68-72g, pappy shell 48-52g, tuber of stemona 4-20g, Cynanchum glaucescens 8-10g, root bark of white mulberry 5.5-6.5g, campanulaceae 5.5-6.5g are thin Lotus brain 0.14-0.16g, citric acid 0.45-0.55g, sucrose 590-610g, sodium benzoate 2.4-2.6g, flavoring banana essence 0.05- 0.10g, ethyl alcohol 0.90-0.97g add purified water constant volume;The preparation method is as follows:
(1) pre-treatment: campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, tuber of stemona traditional Chinese medicine of the five flavours material are sorted, washes and cuts, obtain net medicinal material；
(2) it decocts: net medicinal material campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, pappy shell, tuber of stemona Six-element Chinese medicine is successively put into extraction Tank decocts twice, controls steam pressure≤0.25MPA, and the drinking water of 5.5 times of first time dosing material amounts boils 2 hours, filters； The drinking water of second of 4.5 times of dosing material amount, boils 2 hours, filters；
(3) it is concentrated: decoction liquor is set in double effect concentration tank, control, steam pressure≤0.20MPa, vacuum degree is in -0.040- 0.080MPa, is concentrated under reduced pressure by 60-90 DEG C of temperature, and concentrate is sucked high-order Sandwich pot, is heated to boiling, keeps boiling 30 minutes；
(4) be centrifuged: turn on agitator opens cooling and is water-cooled to 45-50 DEG C, is centrifuged laggard centrifugate through channel separator and stores Tank；
(5) centrifugate decoct: by centrifugate from centrifugation basin in suck interlayer Decocting pot, open steam, control steam pressure≤ 0.20MPa, turn on agitator are heated to boiling, and are kept for slightly boiled 40 minutes, spare；
(6) extracting solution is collected: being opened the cooling extracting solution of cooling water and is transferred in clean container after liquid to be extracted is cooled to 70 DEG C；
(7) it prepares: purified water 300-400mL being added in material-compound tank, control steam pressure≤0.30MPa, open stirring, control Sodium benzoate, sucrose are sucked in material-compound tank by material-compound tank suction pipe valve, suck intensified loquet distillate by vacuum degree≤- 0.10MPa Extracting solution is heated to boiling, and keeps 10-20 minutes slightly boiled, and opening cooling water makes medical fluid be cooled to 45 DEG C or less；Citric acid is added, The mixed solution of the flavoring banana essence and menthol that have been dissolved with ethyl alcohol, stirs and evenly mixs, and stops stirring addition purified water to instruction and matches Amount 1000mL processed, is stirred for mixing；With 300 mesh bag filters by medical filtration to filling；
(8) filling.
Further, the adding manner of sodium benzoate: opening vacuum valve, controls vacuum degree≤- 0.07MPa.
Further, the adding manner of sucrose: sucrose will be poured into clean sugared slot and after completing weighing, opens vacuum Valve controls vacuum degree≤- 0.10MPa, opens material-compound tank suction pipe valve, will be in the sucrose sucking material-compound tank after weighing.
Further, citric acid adding manner: when medical fluid is at 45 DEG C or less, by citric acid from manhole under stirring Place is slowly added to.
Further, menthol, flavoring banana essence adding manner, menthol, flavoring banana essence are poured into clean container, added Enter ethyl alcohol, stirring is until be completely dissolved, when medical fluid is cooled to 45 DEG C or less, by dissolved mixed liquor under stirring from It is slowly added at manhole.
Further, every 1000ml intensified loquet distillate is prepared by following raw material and parts by weight: loguat leaf 69g, small-mouthed jar Grain shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, campanulaceae 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, benzene first Sour sodium 2.5g, flavoring banana essence 0.10g, ethyl alcohol 0.97g add purified water constant volume.
Further, step (4) centrifugation is changed to be enriched with: resulting concentrate is measured at clarifying agent adsorption clarification through 1-3 times Reason, removal filtration obtain removal of impurities liquid,
A. it is enriched with for the first time: removal of impurities liquid is enriched with by macropore weak-type cation exchange resin, it is full with n-butanol-methanol 12:1 It is eluted with solution, flow velocity 4.7mL/min, collects eluent a, obtain filtrate；
B. it is enriched with for second: filtrate obtained by A being enriched with by octadecylsilane chemically bonded silica column, with -0.5% second of acetonitrile-methanol Acid ammonium solution (65:26:9) elution, flow velocity 1.0mL/min collect eluent b, obtain filtrate；
C. third time is enriched with: filtrate obtained by B being enriched with by C8 solid phase extraction column, with the mass percentage concentration 50%- containing NaCl The elution of 80% methanol, flow velocity 5.4mL/min collect eluent c, obtain filtrate；
D. the 4th enrichment: by filtrate obtained by C by high-speed countercurrent chromatography enrichment, with ethyl acetate-tertiary butanol and water system, Volume ratio is 0.5-2: 2-4: 1-10 elution, and flow velocity 1.0mL/min collects eluent d；
E. merge pregnant solution a, b, c, d, solvent is recovered under reduced pressure, it is dry, it is redissolved with water, obtains total enriched substance；
Further, clarifying agent be chitosan, active carbon or diatomite any one or more.
Further, loguat leaf is before decoction by pretreatment: loquat leaf raw material is handled after being crushed, being sieved with liquid nitrogen, Again plus saccharomycete bacterium solution fermentation process 10-20 minutes, then rinsed 2-3 times using clear water, addition by 6~12U/g cellulase, The complex enzyme of 50~90U/g pectase and 5~10U/g trypsase composition reacts 2~4h under the conditions of pH4~6 and sufficiently digests 30-60 minutes, enzyme deactivation after freeze-drying, then carried out decocting operation in next step.
Beneficial effects of the present invention
1, the Corosolic acid content that loguat leaf extracts after pre-treatment step is higher than original technique, and enrichment makes strength after concentration Loquat dew effective component integrally improves 10% or more.
2, product precipitation capacity is reduced
Increase after second extraction, concentration and decoct, centrifugation, decoct step again, the sediment removal in traditional Chinese medicine extraction increases to ten thousand / five or more, the clarity of product is effectively ensured.
3, microbiological hazards are reduced
Original process extracting solution extracts, after second extraction through primary, and there is no creatures-killing step in subsequent step, product occurs Microbiological hazards probability is high, now increases and decocts, centrifugation, decocts step again, the risk that microorganism occurs in product substantially reduces.
4, changing addition raw material sequence keeps mouthfeel more preferable.
Specific embodiment
Form by the following examples is described in further detail above content of the invention again, but should not be by this The range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiment, all technologies based on realization belonging to above content of the present invention It all belongs to the scope of the present invention.
Embodiment 1:
Every 1000ml intensified loquet distillate is prepared by following raw material and parts by weight: loguat leaf 69g, pappy shell 50g, the tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, campanulaceae 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, sodium benzoate 2.5g, banana Essence 0.10g, ethyl alcohol 0.97g add purified water constant volume；
(1) pre-treatment: campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, tuber of stemona traditional Chinese medicine of the five flavours material are sorted, washes and cuts, obtain net medicinal material；
(2) it decocts: net medicinal material campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, pappy shell, tuber of stemona Six-element Chinese medicine is successively put into extraction Tank decocts twice, controls steam pressure 0.15MPA, and the drinking water of 5.5 times of first time dosing material amounts boils 2 hours, filters；The The drinking water of 4.5 times of secondary dosing material amounts, boils 2 hours, filters；
(3) it is concentrated: decoction liquor is set in double effect concentration tank, control steam pressure 0.10MPa, vacuum degree is in -0.040MPa, temperature It 60 DEG C, is concentrated under reduced pressure, concentrate is sucked into high-order Sandwich pot, is heated to boiling, keeps boiling 30 minutes；
(4) be centrifuged: turn on agitator opens cooling and is water-cooled to 50 DEG C, is centrifuged laggard centrifugation liquid storage tank through channel separator；
(5) centrifugate decocts: centrifugate being sucked interlayer Decocting pot out of centrifugation basin, steam is opened, controls steam pressure 0.10MPa, turn on agitator are heated to boiling, and are kept for slightly boiled 40 minutes, spare；
(6) extracting solution is collected: being opened the cooling extracting solution of cooling water and is transferred in clean container after liquid to be extracted is cooled to 70 DEG C；
(7) it prepares: purified water 400mL being added in material-compound tank, control steam pressure 0.30MPa, open stirring, control vacuum Degree≤- 0.10MPa sucks sodium benzoate, sucrose in material-compound tank by material-compound tank suction pipe valve, and sucking intensified loquet distillate extracts Liquid is heated to boiling, and is kept for slightly boiled 20 minutes, and opening cooling water makes medical fluid be cooled to 45 DEG C or less；Citric acid is added, has used ethyl alcohol The flavoring banana essence of dissolution and the mixed solution of menthol, stir and evenly mix, and stop stirring and purified water is added to instructing amount of preparation 1000mL is stirred for mixing, with 300 mesh bag filters by medical filtration to filling；
(8) filling.
Wherein: the adding manner of sodium benzoate: opening vacuum valve, controls vacuum degree≤- 0.07MPa；
Wherein: the adding manner of sucrose: sucrose will be poured into clean sugared slot and after completing weighing, open vacuum valve, control Vacuum degree≤- 0.10MPa opens material-compound tank suction pipe valve, will be in the sucrose sucking material-compound tank after weighing；
Wherein: citric acid adding manner: when medical fluid is at 45 DEG C or less, citric acid slowly being added at manhole under stirring Enter；
Wherein: menthol, flavoring banana essence adding manner pour into menthol, flavoring banana essence in clean container, and ethyl alcohol is added, stirs It mixes up to being completely dissolved, it is when medical fluid is cooled to 45 DEG C or less, dissolved mixed liquor is slow at manhole under stirring It is slow to be added.
Embodiment 2:
A kind of preparation method of intensified loquet distillate, every 1000ml intensified loquet distillate are prepared by following raw material and parts by weight: Loguat leaf 69g, pappy shell 50g, tuber of stemona 6g, Cynanchum glaucescens 8g, root bark of white mulberry 5.5g, campanulaceae 6.5g, menthol 0.16g, citric acid 0.55g, sucrose 590g, sodium benzoate 2.6g, flavoring banana essence 0.10g, ethyl alcohol 0.95g add purified water constant volume;
(1) pre-treatment: campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, tuber of stemona traditional Chinese medicine of the five flavours material are sorted, washes and cuts, obtain net medicinal material；
(2) it decocts: net medicinal material campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, pappy shell, tuber of stemona Six-element Chinese medicine is successively put into extraction Tank decocts twice, controls steam pressure 0.25MPA, and the drinking water of 5.5 times of first time dosing material amounts boils 2 hours, filters；The The drinking water of 4.5 times of secondary dosing material amounts, boils 2 hours, filters；
(3) it is concentrated: decoction liquor is set in double effect concentration tank, control, steam pressure 0.20MPa, vacuum degree is in -0.060MPa, temperature 90 DEG C of degree is concentrated under reduced pressure, and concentrate is sucked high-order Sandwich pot, is heated to boiling, keeps boiling 30 minutes；
(4) be centrifuged: turn on agitator opens cooling and is water-cooled to 50 DEG C, is centrifuged laggard centrifugation liquid storage tank through channel separator；
(5) centrifugate decocts: centrifugate being sucked interlayer Decocting pot out of centrifugation basin, opens steam (control steam pressure 0.20MPa, turn on agitator are heated to boiling, and are kept for slightly boiled 40 minutes, spare；
(6) extracting solution is collected: being opened the cooling extracting solution of cooling water and is transferred in clean container after liquid to be extracted is cooled to 70 DEG C；
(7) it prepares: purified water 350mL being added in material-compound tank, control steam pressure 0.20MPa, open stirring, control vacuum degree ≤ -0.10MPa sucks sodium benzoate, sucrose in material-compound tank by material-compound tank suction pipe valve, and sucking intensified loquet distillate extracts Liquid is heated to boiling, and is kept for slightly boiled 15 minutes, and opening cooling water makes medical fluid be cooled to 45 DEG C or less；Citric acid is added, has used ethyl alcohol The flavoring banana essence of dissolution and the mixed solution of menthol, stir and evenly mix, and stop stirring and purified water is added to instructing amount of preparation 1000mL is stirred for mixing, with 300 mesh bag filters by medical filtration to filling；
(8) filling.
Wherein: the adding manner of sodium benzoate: opening vacuum valve, controls vacuum degree≤- 0.07MPa；
Wherein: the adding manner of sucrose: sucrose will be poured into clean sugared slot and after completing weighing, open vacuum valve, control Vacuum degree≤- 0.10MPa opens material-compound tank suction pipe valve, will be in the sucrose sucking material-compound tank after weighing；
Wherein: citric acid adding manner: when medical fluid is at 45 DEG C or less, citric acid slowly being added at manhole under stirring Enter；
Wherein: menthol, flavoring banana essence adding manner pour into menthol, flavoring banana essence in clean container, and ethyl alcohol is added, stirs It mixes until being completely dissolved；It is when medical fluid is cooled to 45 DEG C or less, dissolved mixed liquor is slow at manhole under stirring It is slow to be added.
Embodiment 3:
A kind of preparation method of intensified loquet distillate, every 1000ml intensified loquet distillate are prepared by following raw material and parts by weight: Loguat leaf 72g, pappy shell 52g, tuber of stemona 20g, Cynanchum glaucescens 10g, root bark of white mulberry 6.5g, campanulaceae 5.5g, menthol 0.16g, citric acid 0.45g, sucrose 590g, sodium benzoate 2.4g, flavoring banana essence 0.05g, ethyl alcohol 0.95g add purified water constant volume;
(1) pre-treatment: campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, tuber of stemona traditional Chinese medicine of the five flavours material are sorted, washes and cuts, obtain net medicinal material；
(2) it decocts: net medicinal material campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, pappy shell, tuber of stemona Six-element Chinese medicine is successively put into extraction Tank decocts twice, controls steam pressure 0.25MPa, and the drinking water of 5.5 times of first time dosing material amounts boils 2 hours, filters；The The drinking water of 4.5 times of secondary dosing material amounts, boils 2 hours, filters；
(3) it is concentrated: decoction liquor is set in double effect concentration tank, control, steam pressure 0.20MPa, vacuum degree is in -0.080MPa, temperature 80 DEG C of degree is concentrated under reduced pressure, and concentrate is sucked high-order Sandwich pot, is heated to boiling, keeps boiling 30 minutes；
(4) be centrifuged: turn on agitator opens cooling and is water-cooled to 50 DEG C, is centrifuged laggard centrifugation liquid storage tank through channel separator；
(5) centrifugate decocts: centrifugate being sucked interlayer Decocting pot out of centrifugation basin, steam is opened, controls steam pressure 0.20MPa, turn on agitator are heated to boiling, and are kept for slightly boiled 40 minutes, spare；
(6) extracting solution is collected: being opened the cooling extracting solution of cooling water and is transferred in clean container after liquid to be extracted is cooled to 70 DEG C；
(7) it prepares: purified water 300mL being added in material-compound tank, control steam pressure 0.30MPa, open stirring, control vacuum degree ≤ -0.10MPa sucks sodium benzoate, sucrose in material-compound tank by material-compound tank suction pipe valve, and sucking intensified loquet distillate extracts Liquid is heated to boiling, and is kept for slightly boiled 20 minutes, and opening cooling water makes medical fluid be cooled to 45 DEG C or less；Citric acid is added, and has used second The flavoring banana essence of alcohol dissolution and the mixed solution of menthol, stir and evenly mix, and stop stirring and purified water is added to instructing amount of preparation 1000mL is stirred for mixing, with 300 mesh bag filters by medical filtration to filling；
(8) filling.
Wherein: the adding manner of sodium benzoate: opening vacuum valve, controls vacuum degree≤- 0.07MPa；
Wherein: the adding manner of sucrose: sucrose being poured into clean sugared slot and after completing weighing, opens vacuum valve, and control is true Reciprocal of duty cycle≤- 0.10MPa opens material-compound tank suction pipe valve, will be in the sucrose sucking material-compound tank after weighing；Wherein: citric acid is added Mode: when medical fluid is at 45 DEG C or less, citric acid is slowly added at manhole under stirring；
Wherein: menthol, flavoring banana essence adding manner pour into menthol, flavoring banana essence in clean container, and ethyl alcohol is added, stirs It mixes until being completely dissolved；It is when medical fluid is cooled to 45 DEG C or less, dissolved mixed liquor is slow at manhole under stirring It is slow to be added.
Embodiment 4: every 1000ml intensified loquet distillate is prepared by following raw material and parts by weight: loguat leaf 69g, opium poppy Shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, campanulaceae 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, benzoic acid Sodium 2.5g, flavoring banana essence 0.10g, ethyl alcohol 0.97g add purified water constant volume；
(1) loguat leaf pre-processes: loquat leaf raw material is handled after being crushed, being sieved with liquid nitrogen, then plus saccharomycete bacterium solution fermentation process It 20 minutes, is then rinsed 3 times using clear water, addition is by 12U/g cellulase, 50U/g pectase and 10U/g trypsase composition Complex enzyme, under the conditions of pH6 react 4h sufficiently digest 30 minutes, enzyme deactivation, after freeze-drying, then carry out in next step decoct grasp Make；Remaining is the same as embodiment 1.
Embodiment 5: every 1000ml intensified loquet distillate is prepared by following raw material and parts by weight: loguat leaf 69g, opium poppy Shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, campanulaceae 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, benzoic acid Sodium 2.5g, flavoring banana essence 0.10g, ethyl alcohol 0.97g add purified water constant volume；
Step (4) centrifugation is changed to be enriched with: resulting concentrate is handled through 3 times of amount clarifying agent adsorption clarifications, and removal filtration must be removed Miscellaneous liquid,
A. it is enriched with for the first time: removal of impurities liquid is enriched with by macropore weak-type cation exchange resin, it is full with n-butanol-methanol 12:1 It is eluted with solution, flow velocity 4.7mL/min, collects eluent a, obtain filtrate；
B. it is enriched with for second: filtrate obtained by A being enriched with by octadecylsilane chemically bonded silica column, with -0.5% second of acetonitrile-methanol Acid ammonium solution (65:26:9) elution, flow velocity 1.0mL/min collect eluent b, obtain filtrate；
C. third time is enriched with: filtrate obtained by B being enriched with by C8 solid phase extraction column, with the mass percentage concentration 50% containing NaCl Methanol elution, flow velocity 5.4mL/min collect eluent c, obtain filtrate；
D. the 4th enrichment: by filtrate obtained by C by high-speed countercurrent chromatography enrichment, with ethyl acetate-tertiary butanol and water system, Volume ratio is 2: 2: 1 elutions, and flow velocity 1.0mL/min collects eluent d；
E. merge pregnant solution a, b, c, d, solvent is recovered under reduced pressure, it is dry, it is redissolved with water, obtains total enriched substance；
Clarifying agent is chitosan, remaining is the same as embodiment 1.
Embodiment 6: every 1000ml intensified loquet distillate is prepared by following raw material and parts by weight: loguat leaf 69g, opium poppy Shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, campanulaceae 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, benzoic acid Sodium 2.5g, flavoring banana essence 0.10g, ethyl alcohol 0.97g add purified water constant volume；
Pre-treatment: campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, tuber of stemona traditional Chinese medicine of the five flavours material are sorted, washes and cuts, obtain net medicinal material；
Loguat leaf is by pretreatment: loquat leaf raw material is handled after being crushed, being sieved with liquid nitrogen, then plus saccharomycete bacterium solution fermentation process It 20 minutes, is then rinsed 3 times using clear water, addition is by 12U/g cellulase, 50U/g pectase and 10U/g trypsase composition Complex enzyme, under the conditions of pH6 react 4h sufficiently digest 30 minutes, enzyme deactivation, after freeze-drying, then carry out in next step decoct grasp Make；
(3) it decocts: net medicinal material campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf enzymolysis liquid, pappy shell, tuber of stemona Six-element Chinese medicine is successively thrown Entering extractor, decoct twice, controls steam pressure 0.15MPA, the drinking water of 5.5 times of first time dosing material amounts boils 2 hours, Filtering；The drinking water of second of 4.5 times of dosing material amount, boils 2 hours, filters；
(4) it is concentrated: decoction liquor is set in double effect concentration tank, control steam pressure 0.10MPa, vacuum degree is in -0.040MPa, temperature It 60 DEG C, is concentrated under reduced pressure, concentrate is sucked into high-order Sandwich pot, is heated to boiling, keeps boiling 30 minutes；
(5) be enriched with after being concentrated: resulting concentrate is handled through 1 times of amount clarifying agent adsorption clarification, and removal filtration obtains removal of impurities liquid,
A. it is enriched with for the first time: removal of impurities liquid is enriched with by macropore weak-type cation exchange resin, it is full with n-butanol-methanol 12:1 It is eluted with solution, flow velocity 4.7mL/min, collects eluent a, obtain filtrate；
B. it is enriched with for second: filtrate obtained by A being enriched with by octadecylsilane chemically bonded silica column, with -0.5% second of acetonitrile-methanol Acid ammonium solution (65:26:9) elution, flow velocity 1.0mL/min collect eluent b, obtain filtrate；
C. third time is enriched with: filtrate obtained by B being enriched with by C8 solid phase extraction column, with the mass percentage concentration 50% containing NaCl Methanol elution, flow velocity 5.4mL/min collect eluent c, obtain filtrate；
D. the 4th enrichment: by filtrate obtained by C by high-speed countercurrent chromatography enrichment, with ethyl acetate-tertiary butanol and water system, Volume ratio is 2: 4: 5 elutions, and flow velocity 1.0mL/min collects eluent d；
E. merge pregnant solution a, b, c, d, solvent is recovered under reduced pressure, it is dry, it is redissolved with water, obtains total enriched substance；
Clarifying agent is diatomite；
(6) pregnant solution decocts: pregnant solution being sucked interlayer Decocting pot out of centrifugation basin, steam is opened, controls steam pressure 0.10MPa, turn on agitator are heated to boiling, and are kept for slightly boiled 40 minutes, spare；
(7) extracting solution is collected: being opened the cooling extracting solution of cooling water and is transferred in clean container after liquid to be extracted is cooled to 70 DEG C；
(8) it prepares: purified water 400mL being added in material-compound tank, control steam pressure 0.30MPa, open stirring, control vacuum Degree≤- 0.10MPa sucks sodium benzoate, sucrose in material-compound tank by material-compound tank suction pipe valve, and sucking intensified loquet distillate extracts Liquid is heated to boiling, and is kept for slightly boiled 20 minutes, and opening cooling water makes medical fluid be cooled to 45 DEG C or less；Citric acid is added, has used ethyl alcohol The flavoring banana essence of dissolution and the mixed solution of menthol, stir and evenly mix, and stop stirring and purified water is added to instructing amount of preparation 1000mL is stirred for mixing, with 300 mesh bag filters by medical filtration to filling；
(9) filling.
Wherein: the adding manner of sodium benzoate: opening vacuum valve, controls vacuum degree≤- 0.07MPa；
Wherein: the adding manner of sucrose: sucrose will be poured into clean sugared slot and after completing weighing, open vacuum valve, control Vacuum degree≤- 0.10MPa opens material-compound tank suction pipe valve, will be in the sucrose sucking material-compound tank after weighing；
Wherein: citric acid adding manner: when medical fluid is at 45 DEG C or less, citric acid slowly being added at manhole under stirring Enter；
Wherein: menthol, flavoring banana essence adding manner pour into menthol, flavoring banana essence in clean container, and ethyl alcohol is added, stirs It mixes up to being completely dissolved, it is when medical fluid is cooled to 45 DEG C or less, dissolved mixed liquor is slow at manhole under stirring It is slow to be added.
Comparative example 1: a kind of preparation method of intensified loquet distillate omits step (4) centrifugation and step (5) centrifugate decocts, Remaining is the same as embodiment 1.
Comparative example 2: a kind of preparation method of intensified loquet distillate omits step (4) centrifugation, remaining is the same as embodiment 1.
Comparative example 3: a kind of preparation method of intensified loquet distillate is omitted step (5) centrifugate and is decocted, remaining is the same as embodiment 1.
Comparative example 4: omit step (4) centrifugation and step (5) centrifugate decoct, step (7) is changed to: with produce sucrose, Sodium benzoate, citric acid, menthol measure essence；Extracting solution made from step (6), heating are added in material-compound tank, unlatching is stirred It mixes, addition sodium benzoate, sucrose are allowed to be uniformly dissolved, and continue heating and boil to 100 DEG C, stop stirring constant temperature 120 minutes, open When stirring is cooled to 55 DEG C or less, citric acid, essence and the menthol dissolved with ethyl alcohol is added, stops stirring plus purified water constant volume To instruction amount of preparation 1000mL, stirring and evenly mixing；It is static, filtration, inspection；Remaining is the same as embodiment 1.
Comparative example 5: a kind of preparation method of intensified loquet distillate, by made from the patent No. " CN201110111681.5 " method Intensified loquet distillate.
Comparative example 6: every 1000ml intensified loquet distillate is prepared by following raw material and parts by weight: loguat leaf 69g, opium poppy Shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, campanulaceae 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, benzoic acid Sodium 2.5g, flavoring banana essence 0.10g, ethyl alcohol 0.97g add purified water constant volume；
Step (4) centrifugation is changed to be enriched with: resulting concentrate is handled through 3 times of amount clarifying agent adsorption clarifications, and removal filtration must be removed Miscellaneous liquid,
A. it is enriched with for the first time: removal of impurities liquid is enriched with by macropore weak-type cation exchange resin, it is full with n-butanol-methanol 10:1 It is eluted with solution, flow velocity 4.7mL/min, collects eluent a, obtain filtrate；
B. it is enriched with for second: filtrate obtained by A being enriched with by octadecylsilane chemically bonded silica column, with -0.5% second of acetonitrile-methanol Acid ammonium solution (52:31:17) elution, flow velocity 1.0mL/min collect eluent b, obtain filtrate；
C. third time is enriched with: filtrate obtained by B being enriched with by C8 solid phase extraction column, with the mass percentage concentration 85% containing NaCl Methanol elution, flow velocity 5.4mL/min collect eluent c, obtain filtrate；
D. the 4th enrichment: by filtrate obtained by C by high-speed countercurrent chromatography enrichment, with ethyl acetate-tertiary butanol and water system, Volume ratio is 3: 3: 12 elutions, and flow velocity 1.0mL/min collects eluent d；
E. merge pregnant solution a, b, c, d, solvent is recovered under reduced pressure, it is dry, it is redissolved with water, obtains total enriched substance；
Clarifying agent is diatomite, remaining is the same as embodiment 1.
Test 1:[assay] Corosolic acid, triterpenic acid total amount shine high performance liquid chromatography (Chinese Pharmacopoeia version in 2015 One VI D of annex) measurement.
Chromatographic condition and system suitability are using octadecylsilane chemically bonded silica as filler；With acetonitrile-methanol- 0.5% ammonium acetate solution (67:12:21) is mobile phase；Detection wavelength is 210nm.Number of theoretical plate should not be low by the calculating of ursolic acid peak In 5000.
The preparation precision of test solution measures this product 20ml, with n-butanol-methanol (10:1, water saturation) mixed solution 4 times (15ml, 15ml, 15m, 20ml) is extracted in strength shaking, is merged n-butanol-methanol (10:1, water saturation) solution, is used n-butanol The water 15ml of saturation is washed, and discards aqueous, is divided and is taken n-butanol liquid, water bath method, and residue adds methanol to make to dissolve and be quantitatively transferred to In 2ml measuring bottle, with methanol dilution to scale, shake up, with (0.45 μm) of miillpore filter filter, take subsequent filtrate to get.
The every 1ml total amount containing triterpene acids loquat leaf of this product is with euscaphic acid, tormentic acid, maslinic acid, Corosolic acid, olive The total amount meter of acid and ursolic acid, must not be less than 3.0 μ g.
Corosolic acid, alkaloids and triterpenic acid overall content are bright by pre-treatment or after enrichment for embodiment 4-6 loguat leaf Aobvious higher than embodiment 1, comparative example 1, the content of comparative example 6, comparative example 6 changes eluent proportion discovery active principle content Content than original technique is lower, illustrates that the technique eluent ratio requirement is stringent, and technique provided by the invention is relatively more preferable, and The content of morphine is declined, still in limits, and 6 content highest of embodiment, overall merit, embodiment 6 is in each finger It is best in mark.
Test 2: sediment removal rate: taking after the dregs of a decoction are weighed respectively after being centrifuged, and sediment removal is calculated in proportion Rate, the results are shown in Table 1.
Test 3: clarity inspection technique: certain density test solution and turbidity standard are set pairing by this genealogy of law respectively Ratio it is turbid in glass tube (internal diameter 15~16mm, flat, tool plug is made with colourless, transparent, neutral hard glass), liquid level Height is 40mm, 5 minutes after turbidity standard preparation, with setting in black background, under diffused light, above opacity tube downwards It observes, compare；Or be vertically arranged under umbrella canopy lamp, illumination 1000lx is observed from horizontal direction, is compared；It is used to check solution Clarity or its muddy degree." clarification " specified in text means that the clarity of test solution is identical to solvent for use, or It is less than No. 0.5 turbidity standard, as a result such as table 1.
Test 4: sweet taste sensory test: the bitter taste for the intensified loquet distillate that above-described embodiment 1-3 and comparative example 1-5 are obtained is covered Effect is as shown in following table: 30 people have carried out taste tests marking to sample, and score is higher, and sweet taste is stronger, as a result such as table 1.
Test 5: thimble test: placing 40 days observation deposited phenomenons under high temperature environment, detect its stability, ties Fruit such as table 1.
Test 6: the content of Corosolic acid is measured using high performance liquid chromatograph in intensified loquet distillate.Determination condition: 1100 type high performance liquid chromatograph of Agilent (DAD diode array detector), Waters Nova-Pak C18 chromatographic column (Φ 3.9 × 150mm, 5 μm), mobile phase are -1% aqueous acetic acid of methanol (88: 12) (V/V), 1.0 mL/min of flow velocity, column temperature 34 DEG C, 20 μ L of sample volume, Detection wavelength is respectively 220nm.
Test sample: precision measures sample 20mL, sets in separatory funnel, ammoniates test solution 0.5mL, is saturated with water n-butanol shaking 5 times (40mL, 40mL, 40mL, 20mL, 20mL), combined extract are extracted, water bath method is dissolved with methanol and is transferred to 10mL In measuring bottle, methanol is added to shake up to scale, cross 0.45 μm of miillpore filter to get.
Table 1
Precipitating removal rate is to count very much.
Embodiment 1-3, which increases centrifugation step, as seen from table reduces sediment, under high temperature environment stands and to occur precipitating Probability is lower,
Test 6: microbial limit and risk inspection
Still there are some microorganisms of a small number of product residues in prior art, after individual product places a period of time, especially summer It having will appear fermentation in the season higher situation of room temperature, produced gas physiological phenomenon, the gas generated in air-tight bottle cannot discharge, because And the bottle that occurs rising even rises brokenly by bottle situation, therefore microbial limit and risk inspection are carried out to intensified loquet distillate, by " in State's pharmacopeia " version four requirements in 2015 years, with pseudomonas aeruginosa, Bacillus subtillis, staphylococcus aureus, black-koji mould and Candida albicans carries out methodology validation to intensified loquet distillate microbial decolorization, and embodiment 1-3 and comparative example are produced Intensified loquet distillate respectively take 100 bottles to place 30 days, 60 days, 90 days, 180 days under summer high temperature, as a comparison with 0 day, respectively Aerobic bacteria sum, yeast and mold sum, escherichia coli number are detected, one group of data is respectively randomly selected, as a result such as following table.
There is not bottle phenomenon that rises in 100 bottles in embodiment 1-3 in experimental result, and comparative example 1,5 occurs 2 bottles respectively and rises There is 1 bottle of bottle that rises respectively in bottle, comparative example 2,3, and bottle phenomenon that rises does not occur in comparative example 4, it is known that intensified loquet obtained by embodiment Dew stability significantly improves, and embodiment quality stability is more preferably under same high temperature environment.And the above test result shows to pass through Increasing after second extraction, concentration and decocts, centrifugation, decocts step again, the removal of sediment in traditional Chinese medicine extraction increases to ten thousand/ Five or more, the clarity of product is effectively ensured, and embodiment 1-3 more preferable than the mouthfeel of comparative example 1-5, to intensified loquet distillate The risk of microbial decolorization discovery, the growth of embodiment 1-3 microorganism is lower, eliminates after decocting again after centrifugation big Part microorganism, embodiment 1-3 is more stable under 180 days hot environments, and the probability for the bottle that occurs rising is lower, and in comparative example Microorganism, which does not remove completely, causes comparative example 2 bottle phenomenon that rises occur, and illustrates that comparative example still has microbiological hazards, the present invention Increase on the basis of original technology and decoct, centrifugation, decoct step again, original technology indices meet national standard, still A small amount of atrament precipitating is tended to have in storage, influences user's sense organ, the present invention is to be further improved on this basis, Reduce atrament precipitating, while reducing the risk of microorganism, keeps technical standard more perfect.

Claims (9)

1. a kind of preparation method of intensified loquet distillate, it is characterised in that: every 1000ml intensified loquet distillate is by following raw material and again Amount part is prepared: loguat leaf 68-72g, pappy shell 48-52g, tuber of stemona 4-20g, Cynanchum glaucescens 8-10g, root bark of white mulberry 5.5-6.5g, tangerine Obstruct 5.5-6.5g, menthol 0.14-0.16g, citric acid 0.45-0.55g, sucrose 590-610g, sodium benzoate 2.4-2.6g, it is fragrant Any of several broadleaf plants essence 0.05-0.10g, ethyl alcohol 0.90-0.97g add purified water constant volume;
The preparation method is as follows:
(1) pre-treatment: campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, tuber of stemona traditional Chinese medicine of the five flavours material are sorted, washes and cuts, obtain net medicinal material；
(2) it decocts: net medicinal material campanulaceae, Cynanchum glaucescens, the root bark of white mulberry, loguat leaf, pappy shell, tuber of stemona Six-element Chinese medicine is successively put into extraction Tank decocts twice, controls steam pressure≤0.25MPa, and the drinking water of 5.5 times of first time dosing material amounts boils 2 hours, filters； The drinking water of second of 4.5 times of dosing material amount, boils 2 hours, filters, and merges decoction liquor；
(3) it is concentrated: decoction liquor is set in double effect concentration tank, control steam pressure≤0.20MPa, vacuum degree is in -0.040- 0.080MPa, is concentrated under reduced pressure by 60-90 DEG C of temperature, and concentrate is sucked high-order Sandwich pot, is heated to boiling, keeps boiling 30 minutes；
(4) be centrifuged: turn on agitator opens cooling and is water-cooled to 45-50 DEG C, is centrifuged laggard centrifugate through channel separator and stores Tank；
(5) centrifugate decoct: by centrifugate from centrifugation basin in suck interlayer Decocting pot, open steam, control steam pressure≤ 0.20MPa, turn on agitator are heated to boiling, and are kept for slightly boiled 40 minutes, spare;
(6) extracting solution is collected: being opened the cooling extracting solution of cooling water and is transferred in clean container after liquid to be extracted is cooled to 70 DEG C；
(7) it prepares: purified water 300-400mL being added in material-compound tank, control steam pressure≤0.30MPa, open stirring, control Sodium benzoate, sucrose are sucked in material-compound tank by material-compound tank suction pipe valve, suck intensified loquet distillate by vacuum degree≤- 0.10MPa Extracting solution is heated to boiling, and keeps 10-20 minutes slightly boiled, and opening cooling water makes medical fluid be cooled to 45 DEG C or less；Citric acid is added, It with the flavoring banana essence of ethyl alcohol dissolution and the mixed solution of menthol, stirs and evenly mixs, stops stirring and purified water is added to extremely instruction Amount of preparation 1000mL is stirred for mixing；With 300 mesh bag filters by medical filtration to filling；
It is filling.
2. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that the addition side of sodium benzoate Formula: opening vacuum valve, controls vacuum degree≤- 0.07MPa.
3. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that the adding manner of sucrose: Sucrose is poured into clean sugared slot and after completing weighing, open vacuum valve, control vacuum degree≤- 0.10MPa, opens material-compound tank Suction pipe valve, will be in the sucrose sucking material-compound tank after weighing.
4. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that citric acid adding manner: When medical fluid is at 45 DEG C or less, citric acid is slowly added at manhole under stirring.
5. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that menthol, flavoring banana essence Adding manner pours into menthol, flavoring banana essence in clean container, ethyl alcohol is added, stirring is until be completely dissolved；When medical fluid is cooling When to 45 DEG C or less, dissolved mixed liquor is slowly added at manhole under stirring.
6. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that every 1000ml intensified loquet Dew is prepared by following raw material and parts by weight: loguat leaf 69g, pappy shell 50g, tuber of stemona 15g, Cynanchum glaucescens 9g, root bark of white mulberry 6g, tangerine Obstruct 6g, menthol 0.15g, citric acid 0.49g, sucrose 600g, sodium benzoate 2.5g, flavoring banana essence 0.10g, ethyl alcohol 0.97g add Purified water constant volume.
7. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that change step (4) centrifugation For enrichment: resulting concentrate is measured clarifying agent adsorption clarification through 1-3 times and is handled, and removal filtration obtains removal of impurities liquid,
A. it is enriched with for the first time: removal of impurities liquid is enriched with by macropore weak-type cation exchange resin, it is full with n-butanol-methanol 12:1 It is eluted with solution, flow velocity 4.7mL/min, collects eluent a, obtain filtrate；
B. it is enriched with for second: filtrate obtained by A being enriched with by octadecylsilane chemically bonded silica column, with -0.5% second of acetonitrile-methanol Acid ammonium solution (65:26:9) elution, flow velocity 1.0mL/min collect eluent b, obtain filtrate；
C. third time is enriched with: filtrate obtained by B being enriched with by C8 solid phase extraction column, with the mass percentage concentration 50%- containing NaCl The elution of 80% methanol, flow velocity 5.4mL/min collect eluent c, obtain filtrate；
D. the 4th enrichment: by filtrate obtained by C by high-speed countercurrent chromatography enrichment, with ethyl acetate-tertiary butanol and water system, Volume ratio is 0.5-2: 2-4: 1-10 elution, and flow velocity 1.0mL/min collects eluent d；
E. merge pregnant solution a, b, c, d, solvent is recovered under reduced pressure, it is dry, it is redissolved with water, obtains total enriched substance.
8. a kind of preparation method of intensified loquet distillate according to claim 7, which is characterized in that clarifying agent be chitosan, Active carbon or diatomite any one or more.
9. a kind of preparation method of intensified loquet distillate according to claim 1, which is characterized in that loguat leaf is passed through before decoction Cross pretreatment: loquat leaf raw material is handled after being crushed, being sieved with liquid nitrogen, then plus saccharomycete bacterium solution fermentation process 10-20 minutes, so It is rinsed 2-3 times, is added by 6~12U/g cellulase, 50~90U/g pectase and 5~10U/g trypsase using clear water afterwards The complex enzyme of composition reacts 2~4h under the conditions of pH4~6 and sufficiently digests 30-60 minutes, and enzyme deactivation after freeze-drying, then carries out Operation is decocted in next step.
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Cited By (5)

* Cited by examiner, † Cited by third party
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CN111529648A (en) * 2020-05-26 2020-08-14 哈尔滨市康隆药业有限责任公司 Low-sugar type taste-masking drug-loading system for carrying traditional Chinese medicine composition and low-sugar type strong loquat syrup
CN111529648B (en) * 2020-05-26 2021-11-19 哈尔滨市康隆药业有限责任公司 Low-sugar type taste-masking drug-loading system for carrying traditional Chinese medicine composition and low-sugar type strong loquat syrup
CN113009040A (en) * 2021-03-15 2021-06-22 玉林市食品药品检验检测中心 Detection method of fingerprint of strong loquat syrup and fingerprint thereof
CN113009040B (en) * 2021-03-15 2022-10-04 玉林市食品药品检验检测中心 Detection method of fingerprint of strong loquat syrup and fingerprint thereof
CN115381060A (en) * 2021-05-24 2022-11-25 福建省神蜂科技开发有限公司 Throat-moistening and lung-nourishing honey loquat leaf extract and preparation method thereof
CN114146147A (en) * 2021-12-13 2022-03-08 中峘本草制药有限公司 Method for uniformly mixing strong loquat syrup
CN115845006A (en) * 2022-12-05 2023-03-28 哈尔滨市康隆药业有限责任公司 Preparation method of strong loquat syrup

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