CN109125258B - Preparation method of strong loquat syrup - Google Patents
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Abstract
The invention provides a preparation method of strong loquat syrup, which comprises the steps of adding water to six ingredients such as loquat leaves and the like in a formula except menthol, decocting twice, each time lasting 2 hours, combining decoction, filtering, concentrating, centrifuging, decocting centrifugate, and concentrating for enrichment, so that the effective components of the strong loquat syrup are integrally improved.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicine pharmacy, and particularly relates to a preparation method of strong loquat syrup.
Background
Strong loquat dew is light brown clear liquid; fragrant and sweet. To nourish yin, astringe lung, relieve cough and dispel phlegm. Can be used for treating cough due to bronchitis. The main ingredients are folium Eriobotryae, plantula Papaveris, radix Stemonae, rhizoma Cynanchi Stauntonii, cortex Mori, radix Platycodi, and Mentholum. Loquat leaf and mulberry bark clear away the lung-heat, stemona root moistens the lung, poppy shell astringes the lung, platycodon root diffuses the lung, and cynanchum glaucescens descends the lung. The functional indications are as follows: nourish yin, astringe lung, relieve cough and eliminate phlegm. Can be used for treating chronic cough, bronchitis, etc.
The invention relates to a strong loquat syrup and a preparation method thereof, as in CN200510010324.4 in the prior art, seven Chinese medicines of loquat leaves and the like, except menthol, other six Chinese medicines of loquat leaves and the like are decocted with water twice, each time lasts for 2 hours, decoction liquids are merged, filtered and concentrated until the relative density of the liquid medicine is 1.13 to 1.15, 2g of steviosin is added for dissolution, 0.5g of citric acid is added, a proper amount of essence and menthol are dissolved by ethanol, and the preparation method is obtained after stirring, uniformly mixing, standing, filtering, adding water to 1000ml and uniformly mixing. For example, in CN201110111681.5, the weight ratio g of the strong loquat syrup is as follows: 50g of loquat leaves, 45g of poppy shells, 10g of radix stemonae, 6g of cynanchum glaucescens, 4g of white mulberry root-bark, 4g of platycodon grandiflorum and 0.09g of menthol; the preparation method comprises decocting the rest six materials except menthol with water twice for 2.5 hr each time, mixing decoctions, filtering, concentrating to 700ml, adding sodium benzoate 2.6g, stirring to dissolve, adding sucrose 700g, heating to boil, keeping the temperature for 30 min, standing, filtering, adding water to 1200ml, and mixing. The technology is basically prepared by secondary decoction, filtration and concentration, but practice proves that the strong loquat syrup prepared by the method has little black substance precipitation after being found for a long time in the storage process and is easily influenced by high-temperature illumination, so that the microbial risk is increased, even the bottle is expanded, the high risk is caused, the bitter taste cannot be reduced to meet the requirement of palatability of a user, and because the loquat leaves are the main drug of the strong loquat syrup, because the loquat leaf components in each production place are slightly different, according to the modern industrialized planting requirement of the loquat leaves and the growth characteristics of the loquat leaves, a large amount of pruned loquat leaves or naturally withered loquat leaves generated in the loquat planting process are used as raw materials, the effective components of the loquat leaves stored for a long time tend to be reduced, and in addition, the tendency of product degradation in the loquat leaf planting process causes the content of the effective components in the loquat leaves to be reduced, the content of the effective components extracted by the traditional process is insufficient, concentration enrichment or wall breaking pretreatment is possibly needed to enable the effective substances to reach the proper content, and the triterpenic acid components such as corosolic acid, rosanic acid and the like belong to the effective components. Therefore, there is no reference in patent and non-patent documents that disclose the improvement of clarity, the improvement of effective substance content of main drug and the reduction of risk of microorganisms, and the technical solutions to be described below are generated under such circumstances.
Disclosure of Invention
Aiming at the problems of low extraction rate of effective components of loquat leaves and precipitation risk and microorganism risk of strong loquat dew products in the traditional process, the problems are effectively solved in the process by adding the procedures of decoction of concentrated solution, centrifugation after decoction, decoction again after centrifugation and the like or enrichment after concentration and the pretreatment process of loquat leaf wall breaking in the production process.
The invention aims to provide a preparation method of strong loquat syrup, which increases the steps of centrifugation and decoction of centrifugate to reduce the risk of precipitation and microorganisms, and also aims to provide a pretreatment method of main drug loquat leaves to ensure that the loquat leaves are extracted more completely, and provide a concentrated solution enrichment method to ensure that the content of active substances of the whole strong loquat syrup is increased, in particular to the enrichment of active ingredients of triterpenic acid in the loquat leaves.
The purpose of the invention is realized by the following technical scheme:
a preparation method of strong loquat syrup is characterized in that each 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 68-72g of loquat leaves, 48-52g of poppy shells, 4-20g of radix stemonae, 8-10g of cynanchum glaucescens, 5.5-6.5g of white mulberry root-bark, 5.5-6.5g of platycodon grandiflorum, 0.14-0.16g of menthol, 0.45-0.55g of citric acid, 610g of cane sugar 590-containing materials, 2.4-2.6g of sodium benzoate, 0.05-0.10g of banana essence, 0.90-0.97g of ethanol, and purified constant volume water, wherein the preparation method comprises the following steps:
(1) pretreatment: selecting five Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves and radix stemonae, washing and cutting to obtain clean medicinal materials;
(2) decocting: sequentially putting clean medicinal materials of six Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves, poppy shells and radix stemonae into an extraction tank, decocting twice, controlling steam pressure to be less than or equal to 0.25MPA, adding drinking water in an amount which is 5.5 times that of the medicinal materials for the first time, boiling for 2 hours, and filtering; adding 4.5 times of drinking water, boiling for 2 hr, and filtering;
(3) concentration: placing the decoction in a double-effect concentration tank, controlling the steam pressure to be less than or equal to 0.20MPa, the vacuum degree to be-0.040-0.080 MPa, the temperature to be 60-90 ℃, concentrating under reduced pressure, sucking the concentrated solution into a high-position interlayer tank, heating to boil, and keeping boiling for 30 minutes;
(4) centrifuging: starting the stirrer, starting cooling water to cool to 45-50 ℃, centrifuging by a tubular separator and then feeding the centrifuged liquid into a centrifugate storage tank;
(5) decocting a centrifugal liquid: sucking the centrifugate from a centrifugal storage tank into an interlayer decocting tank, starting steam, controlling the steam pressure to be less than or equal to 0.20MPa, starting a stirrer, heating to boil, and keeping slight boiling for 40 minutes for later use;
(6) collecting an extracting solution: opening cooling water to cool the extracting solution, and transferring the extracting solution into a clean container after the extracting solution is cooled to 70 ℃;
(7) adding purified water 300-; adding citric acid, the mixed solution of banana essence and menthol dissolved by ethanol, stirring uniformly, stopping stirring, adding purified water to the instruction preparation amount of 1000mL, and stirring uniformly; filtering the liquid medicine by using a 300-mesh bag filter until the liquid medicine is filled;
(8) and (6) filling.
Further, the adding mode of sodium benzoate is as follows: opening the vacuum valve, and controlling the vacuum degree to be less than or equal to-0.07 MPa.
Further, the adding mode of the sucrose is as follows: pouring the sucrose into a clean sugar tank, weighing, opening a vacuum valve, controlling the vacuum degree to be less than or equal to-0.10 MPa, opening a material suction pipe valve of the batching tank, and sucking the weighed sucrose into the batching tank.
Further, citric acid is added slowly from manhole under stirring when the medicinal liquid is below 45 deg.C.
And further, adding the menthol and the banana essence in a mode of pouring the menthol and the banana essence into a clean container, adding ethanol, stirring until the menthol and the banana essence are completely dissolved, and slowly adding the dissolved mixed solution from a manhole under a stirring state when the liquid medicine is cooled to below 45 ℃.
Furthermore, every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing.
Further, the centrifugation in the step (4) is changed into enrichment: subjecting the obtained concentrated solution to 1-3 times of clarifier for adsorption and clarification, removing impurities and filtering to obtain impurity-removed solution,
A. first enrichment: and (3) enriching the impurity removal liquid by macroporous weak acid type cation exchange resin, and performing normal butanol-methanol separation by using a solvent of n-butanol-methanol 12: 1, eluting with saturated solution at the flow rate of 4.7mL/min, and collecting eluent a to obtain filtrate;
B. and (3) second enrichment: enriching the filtrate obtained in the step A through an octadecylsilane chemically bonded silica gel column, eluting with acetonitrile-methanol-0.5% ammonium acetate solution (65: 26: 9) at the flow rate of 1.0mL/min, and collecting an eluent b to obtain a filtrate;
C. and (3) enriching for the third time: enriching the filtrate obtained from the step B through a C8 solid phase extraction small column, eluting with methanol containing NaCl with the mass percentage concentration of 50-80%, wherein the flow rate is 5.4mL/min, and collecting an eluent C to obtain a filtrate;
D. fourth enrichment: enriching the filtrate obtained from the step C by high-speed counter-current chromatography, eluting with an ethyl acetate-tert-butanol-water system at a volume ratio of 0.5-2: 2-4: 1-10 and a flow rate of 1.0mL/min, and collecting an eluate d;
E. combining the enriched solutions a, b, c and d, recovering the solvent under reduced pressure, drying, and redissolving with water to obtain a total enriched substance;
further, the clarifying agent is one or more of chitosan, activated carbon or diatomite.
Further, the loquat leaves are pretreated before decoction: the method comprises the steps of crushing and sieving a loquat leaf raw material, treating the loquat leaf raw material with liquid nitrogen, adding yeast liquid for fermentation treatment for 10-20 minutes, washing the loquat leaf raw material for 2-3 times with clear water, adding a complex enzyme consisting of 6-12U/g cellulase, 50-90U/g pectinase and 5-10U/g trypsin, reacting for 2-4 hours under the condition of pH 4-6 for sufficient enzymolysis for 30-60 minutes, inactivating enzyme, freeze-drying, and then carrying out the next decocting operation.
The invention has the advantages of
1. The content of corosolic acid extracted from the pre-treatment step of the loquat leaves is higher than that of the corosolic acid extracted from the loquat leaves in the prior art, and the concentration of the corosolic acid enables the total effective components of the strong loquat dew to be improved by more than 10%.
2. Reduced product precipitation
The steps of decoction, centrifugation and re-decoction are added after the secondary extraction and concentration, the removal of the precipitate in the traditional Chinese medicine extraction is increased to more than five ten-thousandth, and the clarity of the product is effectively ensured.
3. Reducing microbial risk
After primary extraction and secondary extraction are carried out on the extracting solution in the prior art, the step of killing microorganisms is not needed in the subsequent steps, the risk probability of the microorganisms appearing in the product is high, the steps of decoction, centrifugation and re-decoction are added, and the risk of the microorganisms appearing in the product is greatly reduced.
4. The taste is better by changing the sequence of adding raw materials.
Detailed Description
The foregoing aspects of the present invention are described in further detail below by way of examples, but it should not be construed that the scope of the subject matter of the present invention is limited to the following examples, and that all the technologies that can be realized based on the above aspects of the present invention are within the scope of the present invention.
Example 1:
every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing;
(1) pretreatment: selecting five Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves and radix stemonae, washing and cutting to obtain clean medicinal materials;
(2) decocting: sequentially putting clean medicinal materials of six Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves, poppy shells and radix stemonae into an extraction tank, decocting twice, controlling steam pressure to be 0.15MPA, adding drinking water in an amount which is 5.5 times that of the medicinal materials for the first time, boiling for 2 hours, and filtering; adding 4.5 times of drinking water, boiling for 2 hr, and filtering;
(3) concentration: placing the decoction in a double-effect concentration tank, controlling steam pressure at 0.10MPa, vacuum degree at-0.040 MPa, and temperature at 60 deg.C, concentrating under reduced pressure, sucking the concentrated solution into a high-level interlayer tank, heating to boil, and keeping boiling for 30 min;
(4) centrifuging: starting the stirrer, starting cooling water to cool to 50 ℃, centrifuging by a tubular separator and then feeding the centrifuged liquid into a centrifugate storage tank;
(5) decocting a centrifugal liquid: sucking the centrifugate from a centrifugal storage tank into an interlayer decocting tank, starting steam, controlling the steam pressure to be 0.10MPa, starting a stirrer, heating to boil, and keeping slight boiling for 40 minutes for later use;
(6) collecting an extracting solution: opening cooling water to cool the extracting solution, and transferring the extracting solution into a clean container after the extracting solution is cooled to 70 ℃;
(7) adding 400mL of purified water into a blending tank, controlling the steam pressure to be 0.30MPa, starting stirring, controlling the vacuum degree to be less than or equal to-0.10 MPa, sucking sodium benzoate and sucrose into the blending tank through a material sucking pipe valve of the blending tank, sucking strong loquat syrup extracting solution, heating to boil, keeping slightly boiling for 20 minutes, and starting cooling water to cool the liquid medicine to be below 45 ℃; adding citric acid, the mixed solution of banana essence and menthol dissolved by ethanol, stirring uniformly, stopping stirring, adding purified water to the instruction preparation amount of 1000mL, stirring uniformly, filtering the liquid medicine by using a 300-mesh bag filter until filling;
(8) and (6) filling.
Wherein: the addition mode of sodium benzoate: opening a vacuum valve, and controlling the vacuum degree to be less than or equal to-0.07 MPa;
wherein: the adding mode of the sucrose is as follows: pouring sucrose into a clean sugar tank, weighing, opening a vacuum valve, controlling the vacuum degree to be less than or equal to-0.10 MPa, opening a material suction pipe valve of a batching tank, and sucking the weighed sucrose into the batching tank;
wherein: adding citric acid slowly from manhole under stirring when the medicinal liquid is below 45 deg.C;
wherein: adding Mentholum and fructus Musae essence, pouring Mentholum and fructus Musae essence into clean container, adding ethanol, stirring until completely dissolved, cooling to below 45 deg.C, and slowly adding the dissolved mixture from manhole under stirring.
Example 2:
a preparation method of strong loquat syrup is characterized in that each 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 6g of radix stemonae, 8g of cynanchum glaucescens, 5.5g of white mulberry root-bark, 6.5g of platycodon grandiflorum, 0.16g of menthol, 0.55g of citric acid, 590g of cane sugar, 2.6g of sodium benzoate, 0.10g of banana essence and 0.95g of ethanol, and purified water is added for volume fixing;
(1) pretreatment: selecting five Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves and radix stemonae, washing and cutting to obtain clean medicinal materials;
(2) decocting: sequentially putting clean medicinal materials of six Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves, poppy shells and radix stemonae into an extraction tank, decocting twice, controlling steam pressure to be 0.25MPA, adding drinking water in an amount which is 5.5 times that of the medicinal materials for the first time, boiling for 2 hours, and filtering; adding 4.5 times of drinking water, boiling for 2 hr, and filtering;
(3) concentration: placing the decoction in a double-effect concentration tank, controlling the steam pressure to be 0.20MPa, the vacuum degree to be-0.060 MPa, the temperature to be 90 ℃, concentrating under reduced pressure, sucking the concentrated solution into a high-position interlayer tank, heating to boil, and keeping boiling for 30 minutes;
(4) centrifuging: starting the stirrer, starting cooling water to cool to 50 ℃, centrifuging by a tubular separator and then feeding the centrifuged liquid into a centrifugate storage tank;
(5) decocting a centrifugal liquid: sucking the centrifugate from the centrifugal storage tank into the interlayer decocting tank, starting steam (controlling steam pressure at 0.20MPa, starting the stirrer, heating to boil, and keeping slightly boiling for 40 min;
(6) collecting an extracting solution: opening cooling water to cool the extracting solution, and transferring the extracting solution into a clean container after the extracting solution is cooled to 70 ℃;
(7) preparation: adding 350mL of purified water into a blending tank, controlling the steam pressure to be 0.20MPa, starting stirring, controlling the vacuum degree to be less than or equal to-0.10 MPa, sucking sodium benzoate and sucrose into the blending tank through a material suction pipe valve of the blending tank, sucking strong loquat syrup extracting solution, heating to boil, keeping slight boiling for 15 minutes, and starting cooling water to cool the liquid to be below 45 ℃; adding citric acid, the mixed solution of banana essence and menthol dissolved by ethanol, stirring uniformly, stopping stirring, adding purified water to the instruction preparation amount of 1000mL, stirring uniformly, filtering the liquid medicine by using a 300-mesh bag filter until filling;
(8) and (6) filling.
Wherein: the addition mode of sodium benzoate: opening a vacuum valve, and controlling the vacuum degree to be less than or equal to-0.07 MPa;
wherein: the adding mode of the sucrose is as follows: pouring sucrose into a clean sugar tank, weighing, opening a vacuum valve, controlling the vacuum degree to be less than or equal to-0.10 MPa, opening a material suction pipe valve of a batching tank, and sucking the weighed sucrose into the batching tank;
wherein: adding citric acid slowly from manhole under stirring when the medicinal liquid is below 45 deg.C;
wherein: adding menthol and banana essence, pouring the menthol and banana essence into a clean container, adding ethanol, and stirring until the menthol and banana essence are completely dissolved; when the liquid medicine is cooled to below 45 ℃, the dissolved mixed liquid is slowly added from a manhole under the stirring state.
Example 3:
a preparation method of strong loquat syrup is characterized in that each 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 72g of loquat leaves, 52g of poppy shells, 20g of radix stemonae, 10g of cynanchum glaucescens, 6.5g of white mulberry root-bark, 5.5g of platycodon grandiflorum, 0.16g of menthol, 0.45g of citric acid, 590g of cane sugar, 2.4g of sodium benzoate, 0.05g of banana essence and 0.95g of ethanol, and purified water is added for volume fixing;
(1) pretreatment: selecting five Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves and radix stemonae, washing and cutting to obtain clean medicinal materials;
(2) decocting: sequentially putting clean medicinal materials of six Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves, poppy capsules and radix stemonae into an extraction tank, decocting twice, controlling the steam pressure to be 0.25MPa, adding drinking water in an amount which is 5.5 times that of the medicinal materials for the first time, boiling for 2 hours, and filtering; adding 4.5 times of drinking water, boiling for 2 hr, and filtering;
(3) concentration: placing the decoction in a double-effect concentration tank, controlling the steam pressure to be 0.20MPa, the vacuum degree to be-0.080 MPa and the temperature to be 80 ℃, concentrating under reduced pressure, sucking the concentrated solution into a high-position interlayer tank, heating to boil, and keeping boiling for 30 minutes;
(4) centrifuging: starting the stirrer, starting cooling water to cool to 50 ℃, centrifuging by a tubular separator and then feeding the centrifuged liquid into a centrifugate storage tank;
(5) decocting a centrifugal liquid: sucking the centrifugate from a centrifugal storage tank into an interlayer decocting tank, starting steam, controlling the steam pressure to be 0.20MPa, starting a stirrer, heating to boil, and keeping slight boiling for 40 minutes for later use;
(6) collecting an extracting solution: opening cooling water to cool the extracting solution, and transferring the extracting solution into a clean container after the extracting solution is cooled to 70 ℃;
(7) preparation: adding 300mL of purified water into a blending tank, controlling the steam pressure to be 0.30MPa, starting stirring, controlling the vacuum degree to be less than or equal to-0.10 MPa, sucking sodium benzoate and sucrose into the blending tank through a material suction pipe valve of the blending tank, sucking strong loquat syrup extracting solution, heating to boil, keeping slight boiling for 20 minutes, and starting cooling water to cool the liquid to be below 45 ℃; adding citric acid, and mixed solution of ethanol-dissolved banana essence and menthol, stirring, stopping stirring, adding purified water to the instruction preparation amount of 1000mL, stirring, filtering with 300 mesh bag filter, and packaging;
(8) and (6) filling.
Wherein: the addition mode of sodium benzoate: opening a vacuum valve, and controlling the vacuum degree to be less than or equal to-0.07 MPa;
wherein: the adding mode of the sucrose is as follows: pouring sucrose into a clean sugar tank, after weighing, opening a vacuum valve, controlling the vacuum degree to be less than or equal to-0.10 MPa, opening a material suction pipe valve of a batching tank, and sucking the weighed sucrose into the batching tank; wherein: adding citric acid slowly from manhole under stirring when the medicinal liquid is below 45 deg.C;
wherein: adding menthol and banana essence, pouring the menthol and banana essence into a clean container, adding ethanol, and stirring until the menthol and banana essence are completely dissolved; when the liquid medicine is cooled to below 45 ℃, the dissolved mixed liquid is slowly added from a manhole under the stirring state.
Example 4: every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing;
(1) pretreating loquat leaves: pulverizing folium Eriobotryae, sieving, treating with liquid nitrogen, adding yeast liquid, fermenting for 20 min, washing with clear water for 3 times, adding complex enzyme composed of 12U/g cellulase, 50U/g pectinase and 10U/g trypsin, reacting for 4 hr under pH6 for 30 min, inactivating enzyme, freeze drying, and decocting; the rest is the same as example 1.
Example 5: every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing;
changing the centrifugation in the step (4) into enrichment: subjecting the obtained concentrated solution to 3 times of clarifying agent for adsorption and clarification, removing impurities and filtering to obtain impurity-removed solution,
A. first enrichment: and (3) enriching the impurity removal liquid by macroporous weak acid type cation exchange resin, and performing normal butanol-methanol separation by using a solvent of n-butanol-methanol 12: 1, eluting with saturated solution at the flow rate of 4.7mL/min, and collecting eluent a to obtain filtrate;
B. and (3) second enrichment: enriching the filtrate obtained in the step A through an octadecylsilane chemically bonded silica gel column, eluting with acetonitrile-methanol-0.5% ammonium acetate solution (65: 26: 9) at the flow rate of 1.0mL/min, and collecting an eluent b to obtain a filtrate;
C. and (3) enriching for the third time: enriching the filtrate obtained from the step B through a C8 solid phase extraction small column, eluting with methanol containing NaCl with the mass percentage concentration of 50%, wherein the flow rate is 5.4mL/min, and collecting an eluent C to obtain a filtrate;
D. fourth enrichment: enriching the filtrate obtained in the step C by high-speed counter-current chromatography, eluting by using an ethyl acetate-tert-butanol-water system with the volume ratio of 2: 1 and the flow rate of 1.0mL/min, and collecting an eluent d;
E. combining the enriched solutions a, b, c and d, recovering the solvent under reduced pressure, drying, and redissolving with water to obtain a total enriched substance;
the clarifying agent was chitosan, as in example 1.
Example 6: every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing;
pretreatment: selecting five Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves and radix stemonae, washing and cutting to obtain clean medicinal materials;
pretreating loquat leaves: pulverizing folium Eriobotryae, sieving, treating with liquid nitrogen, adding yeast liquid, fermenting for 20 min, washing with clear water for 3 times, adding complex enzyme composed of 12U/g cellulase, 50U/g pectinase and 10U/g trypsin, reacting for 4 hr under pH6 for 30 min, inactivating enzyme, freeze drying, and decocting;
(3) decocting: sequentially putting clean medicinal materials of six Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaf enzymolysis liquid, poppy shell and radix stemonae into an extraction tank, decocting twice, controlling steam pressure to be 0.15MPA, adding drinking water in an amount which is 5.5 times that of the medicinal materials for the first time, boiling for 2 hours, and filtering; adding 4.5 times of drinking water, boiling for 2 hr, and filtering;
(4) concentration: placing the decoction in a double-effect concentration tank, controlling steam pressure at 0.10MPa, vacuum degree at-0.040 MPa, and temperature at 60 deg.C, concentrating under reduced pressure, sucking the concentrated solution into a high-level interlayer tank, heating to boil, and keeping boiling for 30 min;
(5) enrichment after concentration: subjecting the obtained concentrated solution to 1 time of clarifier for adsorption and clarification, removing impurities and filtering to obtain impurity-removed solution,
A. first enrichment: and (3) enriching the impurity removal liquid by macroporous weak acid type cation exchange resin, and performing normal butanol-methanol separation by using a solvent of n-butanol-methanol 12: 1, eluting with saturated solution at the flow rate of 4.7mL/min, and collecting eluent a to obtain filtrate;
B. and (3) second enrichment: enriching the filtrate obtained in the step A through an octadecylsilane chemically bonded silica gel column, eluting with acetonitrile-methanol-0.5% ammonium acetate solution (65: 26: 9) at the flow rate of 1.0mL/min, and collecting an eluent b to obtain a filtrate;
C. and (3) enriching for the third time: enriching the filtrate obtained from the step B through a C8 solid phase extraction small column, eluting with methanol containing NaCl with the mass percentage concentration of 50%, wherein the flow rate is 5.4mL/min, and collecting an eluent C to obtain a filtrate;
D. fourth enrichment: enriching the filtrate obtained in the step C by high-speed counter-current chromatography, eluting by using an ethyl acetate-tert-butanol-water system with the volume ratio of 2: 4: 5 and the flow rate of 1.0mL/min, and collecting an eluent d;
E. combining the enriched solutions a, b, c and d, recovering the solvent under reduced pressure, drying, and redissolving with water to obtain a total enriched substance;
the clarifying agent is diatomite;
(6) decocting the enriched liquid: sucking the concentrated solution into an interlayer decocting tank from a centrifugal storage tank, starting steam, controlling the steam pressure to be 0.10MPa, starting a stirrer, heating to boil, and keeping micro-boiling for 40 minutes for later use;
(7) collecting an extracting solution: opening cooling water to cool the extracting solution, and transferring the extracting solution into a clean container after the extracting solution is cooled to 70 ℃;
(8) adding 400mL of purified water into a blending tank, controlling the steam pressure to be 0.30MPa, starting stirring, controlling the vacuum degree to be less than or equal to-0.10 MPa, sucking sodium benzoate and sucrose into the blending tank through a material sucking pipe valve of the blending tank, sucking strong loquat syrup extracting solution, heating to boil, keeping slightly boiling for 20 minutes, and starting cooling water to cool the liquid medicine to be below 45 ℃; adding citric acid, the mixed solution of banana essence and menthol dissolved by ethanol, stirring uniformly, stopping stirring, adding purified water to the instruction preparation amount of 1000mL, stirring uniformly, filtering the liquid medicine by using a 300-mesh bag filter until filling;
(9) and (6) filling.
Wherein: the addition mode of sodium benzoate: opening a vacuum valve, and controlling the vacuum degree to be less than or equal to-0.07 MPa;
wherein: the adding mode of the sucrose is as follows: pouring sucrose into a clean sugar tank, weighing, opening a vacuum valve, controlling the vacuum degree to be less than or equal to-0.10 MPa, opening a material suction pipe valve of a batching tank, and sucking the weighed sucrose into the batching tank;
wherein: adding citric acid slowly from manhole under stirring when the medicinal liquid is below 45 deg.C;
wherein: adding Mentholum and fructus Musae essence, pouring Mentholum and fructus Musae essence into clean container, adding ethanol, stirring until completely dissolved, cooling to below 45 deg.C, and slowly adding the dissolved mixture from manhole under stirring.
Comparative example 1: a method for preparing strong loquat distillate without the centrifugation in step (4) and the decoction in step (5) is as in example 1.
Comparative example 2: a method for preparing strong loquat distillate without centrifugation in step (4) is the same as that in example 1.
Comparative example 3: a method for preparing strong loquat distillate is the same as that of example 1 except that the decoction of the centrifugate in the step (5) is omitted.
Comparative example 4: omitting the centrifugation in the step (4) and the decoction of the centrifuged liquid in the step (5), and changing the step (7) into the following steps: preparing sucrose, sodium benzoate, citric acid and menthol, and measuring essence; adding the extracting solution prepared in the step (6) into a mixing tank, heating, starting stirring, adding sodium benzoate and sucrose to dissolve uniformly, continuing heating and boiling to 100 ℃, stopping stirring, keeping the temperature for 120 minutes, starting stirring, cooling to below 55 ℃, adding citric acid, essence and menthol dissolved by ethanol, stopping stirring, adding purified water to a specified preparation volume of 1000mL, and stirring and mixing uniformly; standing, filtering, and inspecting; the rest is the same as example 1.
Comparative example 5: a preparation method of QIANGLIPIPA distillate is disclosed, which is prepared by the method of patent No. CN 201110111681.5.
Comparative example 6: every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing;
changing the centrifugation in the step (4) into enrichment: subjecting the obtained concentrated solution to 3 times of clarifying agent for adsorption and clarification, removing impurities and filtering to obtain impurity-removed solution,
A. first enrichment: and (3) enriching the impurity removal liquid by macroporous weak acid type cation exchange resin, and performing normal butanol-methanol 10: 1, eluting with saturated solution at the flow rate of 4.7mL/min, and collecting eluent a to obtain filtrate;
B. and (3) second enrichment: enriching the filtrate obtained in the step A through an octadecylsilane chemically bonded silica gel column, eluting with acetonitrile-methanol-0.5% ammonium acetate solution (52: 31: 17) at the flow rate of 1.0mL/min, and collecting an eluent b to obtain a filtrate;
C. and (3) enriching for the third time: enriching the filtrate obtained from the step B through a C8 solid phase extraction small column, eluting with methanol containing NaCl with the mass percentage concentration of 85 percent at the flow rate of 5.4mL/min, and collecting an eluent C to obtain a filtrate;
D. fourth enrichment: enriching the filtrate obtained in the step C by high-speed counter-current chromatography, eluting by using an ethyl acetate-tert-butanol-water system with the volume ratio of 3: 12 and the flow rate of 1.0mL/min, and collecting an eluent d;
E. combining the enriched solutions a, b, c and d, recovering the solvent under reduced pressure, drying, and redissolving with water to obtain a total enriched substance;
the clarifying agent was diatomaceous earth, as in example 1.
Test 1 [ content determination ] the total amount of corosolic acid and triterpenic acid was determined by high performance liquid chromatography (appendix VI D of the first part of the pharmacopoeia 2015, China).
Octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile-methanol-0.5% ammonium acetate solution (67: 12: 21) is used as a mobile phase; the detection wavelength was 210 nm. The number of theoretical plates should not be less than 5000 calculated according to the ursolic acid peak.
Precisely weighing 20ml of the product for preparation of a test solution, strongly shaking and extracting 4 times (15 ml, 15m and 20ml) by using a mixed solution of n-butyl alcohol and methanol (10: 1, water saturation), combining n-butyl alcohol and methanol (10: 1, water saturation), washing by using 15ml of water saturated by n-butyl alcohol, discarding water solution, separately taking n-butyl alcohol solution, evaporating to dryness in water bath, dissolving residue by adding methanol, quantitatively transferring to a 2ml measuring flask, diluting to scale by using methanol, shaking up, filtering by using a microporous filter membrane (0.45 mu m), and taking a subsequent filtrate to obtain the product.
The total content of triterpenic acid in the product per 1ml is not less than 3.0 μ g, based on total amount of Rosa acid, tormentic acid, Maslinic acid, corosolic acid, oleanolic acid and ursolic acid.
Examples 4-6 the total content of corosolic acid, alkaloids and triterpenic acid after the loquat leaves are pretreated or enriched is obviously higher than that of examples 1, 1 and 6, the proportion of the eluent in the comparative example 6 is changed, the content of effective substances is found to be lower than that of the original process, which shows that the proportion requirement of the eluent in the process is strict, the process provided by the invention is relatively better, the content of morphine is reduced to a certain extent and still in the limit range, and the highest content in the example 6 is comprehensively evaluated, and the example 6 is the best in all indexes.
Test 2: removal rate of precipitate: after centrifugation, the residues were weighed respectively, and the removal rate of the precipitate was calculated in proportion, with the results shown in table 1.
Test 3: clarity test method: in the method, a test solution with a certain concentration and a turbidity standard solution are respectively arranged in a turbidity-comparing glass tube (with the inner diameter of 15-16 mm, a flat bottom and a plug, and the turbidity standard solution is made of colorless, transparent and neutral hard glass), the height of the liquid level is 40mm, 5 minutes after the turbidity standard solution is prepared, the turbidity standard solution is arranged on a black background, and the turbidity is observed and compared from the upper part of the turbidity tube downwards under diffused light; or vertically arranged under the canopy lamp, the illumination is 1000lx, and the observation and the comparison are carried out in the horizontal direction; to check the clarity of the solution or its turbidity. The term "clear" as used herein means that the sample solution has the same clarity as the solvent used, or does not exceed the turbidity standard of 0.5, and the results are shown in Table 1.
Test 4: and (3) sweet taste testing: the bitterness masking effect of the strong loquat dew obtained in examples 1 to 3 and comparative examples 1 to 5 is shown in the following table: the samples were scored for taste by 30 people, with higher scores and stronger sweetness, and the results are given in table 1.
Test 5: high temperature stability test: the precipitate was observed after standing at a high temperature for 40 days, and the stability was examined, and the results are shown in Table 1.
Test 6: the content of corosolic acid in the strong loquat syrup is determined by a high performance liquid chromatograph. The measurement conditions were as follows: agilent 1100 type high performance liquid chromatograph (DAD diode array detector), Waters Nova-Pak C18 chromatographic column (phi 3.9 × 150mm, 5 μm), mobile phase methanol-1% acetic acid aqueous solution (88: 12) (V/V), flow rate of 1.0mL/min, column temperature of 34 deg.C, sample injection amount of 20 μ L, and detection wavelength of 220nm respectively.
And (3) testing the sample: precisely measuring 20mL of sample, placing in a separating funnel, adding 0.5mL of ammonia test solution, extracting with water saturated n-butanol under shaking for 5 times (40mL, 20mL), mixing extractive solutions, evaporating in water bath, dissolving with methanol, transferring into a 10mL measuring flask, adding methanol to scale, shaking, and filtering with 0.45 μm microporous membrane to obtain the final product.
TABLE 1
The removal rate of the precipitate is ten thousand.
As can be seen from the table, the addition of the centrifugation step in examples 1 to 3 reduces the precipitate, the precipitation rate is lower when the solution is left standing in a high temperature environment,
test 6: microbial limit and risk check
In the prior art, a few products still have some microorganisms, after individual products are placed for a period of time, particularly, the physiological phenomena of fermentation and gas production can occur under the condition of higher room temperature in summer, and gas generated in a sealed bottle can not be released, so that the situation that the bottle is expanded or even the bottle is expanded is generated, so that the microorganism limit and the risk of the strong loquat dew are checked, according to the requirements of the four parts of the 2015 edition of Chinese pharmacopoeia, a methodological verification is carried out on the microorganism limit checking method of the strong loquat dew by using pseudomonas aeruginosa, bacillus subtilis, staphylococcus aureus, aspergillus niger and candida albicans, 100 bottles of the strong loquat dew produced in examples 1-3 and comparative examples are respectively placed at the high temperature in summer for 30 days, 60 days, 90 days and 180 days, and are compared with 0 day, the total number of aerobic bacteria, the total number of mould and saccharomycetes and the number of escherichia coli are respectively detected, one set of data was randomly selected for each and the results are given in the table below.
In the experimental results, the bottles of examples 1 to 3 did not rise in 100 bottles, the bottles of comparative examples 1 and 5 did not rise in 2 bottles, the bottles of comparative examples 2 and 3 did not rise in 1 bottle, and the bottles of comparative example 4 did not rise in 4 bottles, so that the stability of the strong loquat syrup prepared in the examples was significantly improved, and the quality stability of the examples was better under the same high-temperature environment. And the above test results show that, through adding the steps of decocting, centrifuging and re-decocting after secondary extraction and concentration, the removal of precipitates in the traditional Chinese medicine extraction is increased to more than five per ten thousand, the clarity of the product is effectively ensured, and the mouthfeel of the examples 1-3 is better than that of the examples 1-5, the examination method for the limit of microorganisms of the strong loquat dew shows that the growth risk of the microorganisms of the examples 1-3 is lower, most microorganisms are removed after centrifuging and re-decocting, the examples 1-3 are more stable in a high-temperature environment of 180 days and have lower probability of bottle expansion, the microorganism in the comparative example is not completely removed, so that the bottle expansion phenomenon of the comparative example 2 is caused, and the microbial risk still exists in the comparative example, the steps of decocting, centrifuging and re-decocting are added on the basis of the prior art, and all indexes of the prior art accord with the national standard, but a small amount of black substances are easy to precipitate in storage, which affects the appearance of a user.
Claims (8)
1. A preparation method of strong loquat syrup is characterized by comprising the following steps: every 1000ml of strong loquat syrup is prepared from the following raw materials in parts by weight: 68-72g of loquat leaves, 48-52g of poppy shells, 4-20g of radix stemonae, 8-10g of cynanchum glaucescens, 5.5-6.5g of white mulberry root-bark, 5.5-6.5g of platycodon grandiflorum, 0.14-0.16g of menthol, 0.45-0.55g of citric acid, 610g of sucrose 590-containing materials, 2.4-2.6g of sodium benzoate, 0.05-0.10g of banana essence, 0.90-0.97g of ethanol, and purified constant volume water is added;
the preparation method comprises the following steps:
(1) pretreatment: selecting five Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves and radix stemonae, washing and cutting to obtain clean medicinal materials;
(2) decocting: sequentially putting clean medicinal materials of six Chinese medicinal materials of platycodon grandiflorum, cynanchum glaucescens, cortex mori radicis, loquat leaves, poppy shell and radix stemonae into an extraction tank, decocting twice, controlling the steam pressure to be less than or equal to 0.25MPa, adding drinking water in an amount which is 5.5 times that of the medicinal materials for the first time, boiling for 2 hours, and filtering; adding 4.5 times of drinking water, boiling for 2 hr, filtering, and mixing decoctions;
(3) concentration: placing the decoction in a double-effect concentration tank, controlling steam pressure to be less than or equal to 0.20MPa, vacuum degree to be-0.040-0.080 MPa, temperature to be 60-90 ℃, concentrating under reduced pressure, sucking the concentrated solution into a high-position interlayer tank, heating to boil, and keeping boiling for 30 minutes;
(4) enrichment: subjecting the obtained concentrated solution to 1-3 times of clarifier for adsorption and clarification, removing impurities and filtering to obtain impurity-removed solution,
A. first enrichment: and (3) enriching the impurity removal liquid by macroporous weak acid type cation exchange resin, and performing normal butanol-methanol separation by using a solvent of n-butanol-methanol 12: 1, eluting with saturated solution at the flow rate of 4.7mL/min, and collecting eluent a to obtain filtrate;
B. and (3) second enrichment: enriching the filtrate obtained in the step A by using an octadecylsilane bonded silica gel column, and performing enrichment by using a solvent with a volume ratio of 65: 26: 9, eluting with acetonitrile-methanol-0.5 percent ammonium acetate solution at the flow rate of 1.0mL/min, and collecting eluent b to obtain filtrate;
C. and (3) enriching for the third time: enriching the filtrate obtained from the step B through a C8 solid phase extraction small column, eluting with methanol containing NaCl with the mass percentage concentration of 50-80%, wherein the flow rate is 5.4mL/min, and collecting an eluent C to obtain a filtrate;
D. fourth enrichment: enriching the filtrate obtained from the step C by high-speed counter-current chromatography, eluting with an ethyl acetate-tert-butanol-water system at a volume ratio of 0.5-2: 2-4: 1-10 and a flow rate of 1.0mL/min, and collecting an eluate d;
E. combining the enriched solutions a, b, c and d, recovering the solvent under reduced pressure, drying, and redissolving with water to obtain a total enriched substance;
(5) decocting the enriched liquid: sucking the enrichment liquid into an interlayer decocting tank, starting steam, controlling the steam pressure to be less than or equal to 0.20MPa, starting a stirrer, heating to boil, and keeping slight boiling for 40 minutes for later use;
(6) collecting an extracting solution: opening cooling water to cool the extracting solution, and transferring the extracting solution into a clean container after the extracting solution is cooled to 70 ℃;
(7) preparation: adding 400mL of purified water into a blending tank, controlling the steam pressure to be less than or equal to 0.30MPa, starting stirring, controlling the vacuum degree to be less than or equal to-0.10 MPa, sucking sodium benzoate and cane sugar into the blending tank through a material sucking pipe valve of the blending tank, sucking strong loquat dew extracting solution, heating to boil, keeping slightly boiling for 10-20 minutes, and starting cooling water to cool the liquid medicine to below 45 ℃; adding citric acid, the mixed solution of banana essence and menthol dissolved by ethanol, stirring uniformly, stopping stirring, adding purified water to the instruction preparation amount of 1000mL, and stirring uniformly; filtering the liquid medicine by using a 300-mesh bag filter until the liquid medicine is filled;
and (6) filling.
2. The preparation method of loquat syrup according to claim 1, wherein the sodium benzoate is added in a manner of: opening the vacuum valve, and controlling the vacuum degree to be less than or equal to-0.07 MPa.
3. The preparation method of loquat syrup according to claim 1, wherein the sucrose is added in the following manner: pouring the sucrose into a clean sugar tank, after weighing, opening a vacuum valve, controlling the vacuum degree to be less than or equal to-0.10 MPa, opening a material suction pipe valve of the batching tank, and sucking the weighed sucrose into the batching tank.
4. The preparation method of loquat syrup according to claim 1, wherein the citric acid is added slowly from the inlet hole while stirring the liquid medicine at 45 ℃ or lower.
5. The preparation method of loquat syrup according to claim 1, wherein the menthol and banana essence are added by pouring the menthol and banana essence into a clean container, adding ethanol, and stirring until completely dissolved; when the liquid medicine is cooled to 45 ℃ or below, the dissolved mixture is slowly added from the inlet hole while stirring.
6. The preparation method of loquat syrup according to claim 1, wherein each 1000ml of loquat syrup is prepared from the following raw materials (by weight portion): 69g of loquat leaves, 50g of poppy shells, 15g of radix stemonae, 9g of cynanchum glaucescens, 6g of white mulberry root-bark, 6g of platycodon grandiflorum, 0.15g of menthol, 0.49g of citric acid, 600g of sucrose, 2.5g of sodium benzoate, 0.10g of banana essence and 0.97g of ethanol, and purified water is added for volume fixing.
7. The method for preparing loquat syrup according to claim 1, wherein the clarifying agent is one or more of chitosan, activated carbon and diatomaceous earth.
8. The method of claim 1, wherein the loquat leaves are pre-treated before decoction: the method comprises the steps of crushing and sieving a loquat leaf raw material, treating the loquat leaf raw material with liquid nitrogen, adding yeast liquid for fermentation treatment for 10-20 minutes, washing the loquat leaf raw material for 2-3 times with clear water, adding a complex enzyme consisting of 6-12U/g cellulase, 50-90U/g pectinase and 5-10U/g trypsin, reacting for 2-4 hours under the condition of pH 4-6, inactivating enzyme, freeze-drying, and then carrying out the next decocting operation.
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| 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 |
| 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 |
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| 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 |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050129790A1 (en) * | 2003-11-17 | 2005-06-16 | Folts John D. | Polyphenol-containing stem and vine extracts and methods of use |
| CN101012248A (en) * | 2007-02-02 | 2007-08-08 | 华东理工大学 | Method of separating and concentrating iridoid glycosides and crocin in cape jasmine fruit |
| CN101274953A (en) * | 2008-05-19 | 2008-10-01 | 福州大学 | Method for extracting corosolic acid from plant |
| CN102228515A (en) * | 2011-06-23 | 2011-11-02 | 中南大学 | Separation and enrichment method of total flavones and total alkaloids of Lotus Plumule |
| CN102600247A (en) * | 2012-04-11 | 2012-07-25 | 宁波德沃生物科技有限公司 | Corydalis saxicola bunting alkaloid extract and preparation method thereof, as well as extraction method of dehydrocavidine |
| JP2012213359A (en) * | 2011-03-31 | 2012-11-08 | Inabata Koryo Kk | METHOD FOR PRODUCING FOOD MATERIAL COMPRISING β-CRYPTOXANTHIN-CONTAINING EXTRACT |
| CN103961613A (en) * | 2014-05-07 | 2014-08-06 | 江西百神药业股份有限公司 | Novel preparation method of high-quality loquat syrup |
| US20140271952A1 (en) * | 2013-03-14 | 2014-09-18 | R.J. Reynolds Tobacco Company | Protein-enriched tobacco-derived composition |
| CN106620452A (en) * | 2017-01-06 | 2017-05-10 | 苏州华葆药业股份有限公司 | Method for preparing powerful folium eriobotryae syrup |
| CN107854537A (en) * | 2017-12-22 | 2018-03-30 | 福建康凌谷生物科技有限公司 | A kind of Extractum Folii Eriobotryae Inspissmatum and preparation method thereof |
-
2018
- 2018-10-25 CN CN201811252712.7A patent/CN109125258B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050129790A1 (en) * | 2003-11-17 | 2005-06-16 | Folts John D. | Polyphenol-containing stem and vine extracts and methods of use |
| CN101012248A (en) * | 2007-02-02 | 2007-08-08 | 华东理工大学 | Method of separating and concentrating iridoid glycosides and crocin in cape jasmine fruit |
| CN101274953A (en) * | 2008-05-19 | 2008-10-01 | 福州大学 | Method for extracting corosolic acid from plant |
| JP2012213359A (en) * | 2011-03-31 | 2012-11-08 | Inabata Koryo Kk | METHOD FOR PRODUCING FOOD MATERIAL COMPRISING β-CRYPTOXANTHIN-CONTAINING EXTRACT |
| CN102228515A (en) * | 2011-06-23 | 2011-11-02 | 中南大学 | Separation and enrichment method of total flavones and total alkaloids of Lotus Plumule |
| CN102600247A (en) * | 2012-04-11 | 2012-07-25 | 宁波德沃生物科技有限公司 | Corydalis saxicola bunting alkaloid extract and preparation method thereof, as well as extraction method of dehydrocavidine |
| US20140271952A1 (en) * | 2013-03-14 | 2014-09-18 | R.J. Reynolds Tobacco Company | Protein-enriched tobacco-derived composition |
| CN103961613A (en) * | 2014-05-07 | 2014-08-06 | 江西百神药业股份有限公司 | Novel preparation method of high-quality loquat syrup |
| CN106620452A (en) * | 2017-01-06 | 2017-05-10 | 苏州华葆药业股份有限公司 | Method for preparing powerful folium eriobotryae syrup |
| CN107854537A (en) * | 2017-12-22 | 2018-03-30 | 福建康凌谷生物科技有限公司 | A kind of Extractum Folii Eriobotryae Inspissmatum and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 以枇杷叶为原料提取乌索酸的工艺研究（V）;李开泉等;《宜春学院学报（自然科学）》;20040831;第26卷(第4期);第1-3页 * |
| 枇杷叶总黄酮的富集及其生物活性的研究;林国荣等;《食品科技》;20141231;第39卷(第11期);第233-237页 * |
| 林檎叶化学成分的分离及其提取物的抗菌、抗氧化活性研究;卢静;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20141215(第12期);第E057-39页 * |
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