CN102772490A - Method for preparing paper mulberry staminate inflorescence hard capsule - Google Patents
Method for preparing paper mulberry staminate inflorescence hard capsule Download PDFInfo
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- CN102772490A CN102772490A CN2012102460797A CN201210246079A CN102772490A CN 102772490 A CN102772490 A CN 102772490A CN 2012102460797 A CN2012102460797 A CN 2012102460797A CN 201210246079 A CN201210246079 A CN 201210246079A CN 102772490 A CN102772490 A CN 102772490A
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- broussonetia papyrifera
- staminate inflorescence
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Abstract
The invention discloses a method for preparing a paper mulberry staminate inflorescence hard capsule. The method comprises the following steps: 1, preparing paper mulberry staminate inflorescence flavone extract: weighing a certain mount of paper mulberry staminate inflorescence powder sample, adding 20% ethanol solution into the sample for reflux extraction, filling the extract liquid into a Buchner funnel, carrying out suction filtering by using a vacuum pump, collecting the filtrate, pouring the filtrate into an evaporation flask, separating the ethanol solution out, adding the distilled water into the concentrate to dissolve, pouring the dissolved solution to a centrifuge tube to remove impurities, sucking the supernatant, collecting the supernatant into a volumetric flask, and adding the distilled water to a constant volume; and 2, preparing the paper mulberry staminate inflorescence hard capsule: putting cane sugar, lactose and soluble starch in an oven to be completely dried, grinding the cane sugar and the lactose in a mortar, weighing according to the ratio of paper mulberry staminate inflorescence extract to cane sugar to lactose to starch being 1:1:1:3, adding the ethanol solution into the extract to be uniformly mixed, granulating, then sieving the granules, and packaging the granules which meet the requirements into the hollow capsule after drying and cooling.
Description
Technical field
The present invention relates to a kind of method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule.
Background technology
Broussonetia papyrifera is claimed papermulberry again, and moraceae plants is a kind of deciduous tree, and adaptability is extremely strong, anti-dry and cold, moisture-proof is warm, well developed root system, little disease and pest.It is the very common wild tree of southern area.The Broussonetia papyrifera whole body all is precious, and its branch, leaf, skin, root bark, milk and fruit can be as medicinal or edible raw materials; The staminate inflorescence of Broussonetia papyrifera is a catkin, and female flower is a head inflorescence, contains 17 seed amino acids in the Broussonetia papyrifera staminate inflorescence, and wherein 7 kinds is essential amino acid, and the Broussonetia papyrifera staminate inflorescence also contains Flavonoid substances through measuring.Up to the present, also do not see report about the development and use of the contained medicinal or edible material from soybeans of Broussonetia papyrifera male flower.Therefore, the contained development and use medicinal or edible material from soybeans of Broussonetia papyrifera male flower have broad prospects.
Should develop energetically.Draw the optimum extraction process of flavone through experiment of single factor and orthogonal test, and extracting solution is added an amount of adjuvant, process hard capsule, be easy to preserve, take more easily.
Summary of the invention
The technical problem that the present invention will solve is, a kind of method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule is provided, and is human development and health service with the contained medicinal or edible material from soybeans of development and use Broussonetia papyrifera male flower.
The present invention takes following technical scheme: it may further comprise the steps: it may further comprise the steps: first; Preparation Broussonetia papyrifera staminate inflorescence flavone extractive; Its process is: take by weighing a certain amount of Broussonetia papyrifera staminate inflorescence powder sample, and according to experiment of single factor and Orthogonal Experiment and Design, change flavone extraction conditions; In sample, add the lixiviate that refluxes of 20%～30% alcoholic solution by solid-liquid ratio 1:20, change lixiviating solution over to cloth wet funnel and use vacuum pump to carry out sucking filtration and collect filtrating; Filtrating is gone in the evaporative flask, use Rotary Evaporators that filtrating is carried out concentrating under reduced pressure, isolate alcoholic solution; After ethanol is separated, the concentrate adding distil water is dissolved, lysate moves in the centrifuge tube, centrifugally in centrifuge removes water-fast impurity, draws supernatant with glue head dropper, is collected in the standardize solution measuring bottle adding distil water standardize solution; The second, Broussonetia papyrifera staminate inflorescence extractum preparation: with the flavone extractive of above-mentioned standardize solution, be rotated distillation 2.5h～3.5h, make Broussonetia papyrifera staminate inflorescence extractum; The 3rd, preparation Broussonetia papyrifera staminate inflorescence hard capsule, its process is: at first place baking oven to dry fully sucrose, lactose and soluble starch; Sucrose and lactose grind in mortar; With Broussonetia papyrifera staminate inflorescence extractum: the ratio of sucrose: lactose: starch=1:1:1:3 takes by weighing, and gets 80%～90% alcoholic solution and is added to mixing in the extractum, pelletize as wetting agent; Afterwards granule is sieved, make it pass 10 molecules of interest sieve, do not pass 80 molecules of interest sieve; The granule that will meet above requirement places the baking oven of 85 ℃ of temperature to dry, and is Broussonetia papyrifera staminate inflorescence hard capsule in the Capsules of treating to pack into after particle drying cools off, and puts into shady and cool dry place then and preserves.
In the first step, " taking by weighing a certain amount of Broussonetia papyrifera staminate inflorescence powder sample " is meant the Broussonetia papyrifera staminate inflorescence powder sample that takes by weighing 5g, 10g, 15g or 20g; " be collected in the standardize solution measuring bottle " and be meant in the standardize solution measuring bottle that is collected into 100 mL, 200 mL, 300 mL or 400 mL; The standardize solution measuring bottle at this place is corresponding with the Broussonetia papyrifera staminate inflorescence powder sample weight that takes by weighing respectively.
In the first step, " solid-liquid ratio 1:20 " is meant sample: alcoholic solution=1 g:20mL.
In the first step, the optimum extraction process of flavone is that concentration of alcohol is 20% in the Broussonetia papyrifera staminate inflorescence, and extracting temperature is 85 ℃, and the extraction time of backflow lixiviate is 3h.
In second step, rotary distillation 3h.
In the third step, get 85% alcoholic solution as wetting agent.
Because the Broussonetia papyrifera staminate inflorescence is in great numbers, a considerable number of; The Broussonetia papyrifera staminate inflorescence is that a kind of total sugar content is suitable, and crude fat content is low, and thick protein and total ash content are high, and amino acid contained abundant and A wide selection of colours and designs has the inflorescence that better nutritivity is worth, and the more important thing is that it contains Flavonoid substances; Therefore the application of Broussonetia papyrifera staminate inflorescence has wide value.The Broussonetia papyrifera staminate inflorescence hard capsule of the present invention's preparation has easy to carry, and the characteristics of taking convenience can be brought into play its medicinal or edibility well.Through the configuration corresponding production equipment, can be generalized to industry production to the method for prepared in laboratory Broussonetia papyrifera staminate inflorescence hard capsule fully, for people's nutrition and health service, create more wealth.
The specific embodiment
Embodiments of the invention: experiment of the present invention takes by weighing Broussonetia papyrifera staminate inflorescence powder sample, and once experiment can take by weighing 5g, also can take by weighing 10g, 15g or 20g; The standardize solution measuring bottle of collecting the supernatant use is corresponding with the Broussonetia papyrifera staminate inflorescence powder sample weight that experiment takes by weighing respectively, is respectively the standardize solution measuring bottle of 100 mL, 200 mL, 300 mL or 400 mL.
One. experiment material and instrument
1.1 experimental raw
Cai Jia closes and selects some strain Broussonetia papyrifera Xiong Shu at random in the Guiyang, gathers the Broussonetia papyrifera staminate inflorescence.Oven dry, grind into fine powder is for use.
1.2 experimental apparatus
| The instrument title | Model | Manufacturer |
| The multifunctional food blender | SS-350 | Shunde District, Foshan City holds osmanthus man and becomes electrical apparatus factory |
| The electric heating constant temperature air dry oven | 101-2 | Last sea route reaches the experimental apparatus company limited |
| The digital display thermostat water bath | HH-2 | Shanghai Pudong Physical and Optical Instruments Factory |
| The circulation ability of swimming is used vacuum pump more | SHB-B95 | Zhengzhou Greatwall Scientific Industrial & Trading Co., Ltd. |
| Electronic balance | FA2004N | Shanghai Jing Hai Instr Ltd. |
| The recirculated water vacuum pump | SHZ-ⅢD | Shanghai Yarong Biochemical Instrument Plant |
| Rotary Evaporators | N-1001 | Shanghai lover Instr Ltd. |
| Oil bath pan | OSB-2000 | Shanghai lover Instr Ltd. |
| Centrifuge | 80-2 | Shanghai Pudong Physical and Optical Instruments Factory |
Experiment reagent
Table
experiment reagent
| Reagent name | Model | Manufacturer |
| Boric acid | Analytical pure | Tianjin Bazhou City's chemical industry subsidiary factory of quartzy Clock Factory |
| Hydrochloric acid | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| Potassium ferrocyanide | Analytical pure | Kingsoft, Chengdu chemical reagent company limited |
| Zinc acetate | Analytical pure | Tianjin Xiehe Haopeng Chromatogram Science & Technology Co., Ltd. |
| Glacial acetic acid | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| Copper sulfate | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| Anhydrous sodium sulfate | Analytical pure | Chongqing luxuriant industry chemical reagent company limited |
| Potassium sulfate | Analytical pure | The north, Tianjin day medical chemistry chemical reagent work |
| Methine is blue | Analytical pure | Tianjin Da Mao chemical reagent factory |
| Petroleum ether | Analytical pure, 30 ~ 60 ℃ of boiling ranges | The Tianjin chemical reagent company limited of passing the civil service examinations |
| Glucose | Analytical pure | Chongqing Bei Bei Fine Chemical Works |
| Oxalic acid | Analytical pure | Tianjin recovery development in science and technology company limited |
| Sodium hydroxide | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| Sodium nitrite | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| Aluminum nitrate | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| Dehydrated alcohol | Analytical pure | Chuanjiang River, Chongqing chemical reagent factory |
| The rutin standard substance | Analytical pure | Guizhou enlightening mcroorganism Co., Ltd |
One. experimental technique
2.1 the preparation of Broussonetia papyrifera staminate inflorescence flavone extractive
Accurately take by weighing the Broussonetia papyrifera staminate inflorescence powder sample of 5g; According to experiment of single factor and Orthogonal Experiment and Design; Change flavone extraction conditions; In sample, add Different concentrations of alcohol solution by certain solid-liquid ratio and extract the lixiviate that refluxes under the temperature, after the lixiviate different time, change lixiviating solution over to cloth wet funnel and use vacuum pump to carry out sucking filtration and collection filtrating in difference.Filtrating is gone in the evaporative flask, use Rotary Evaporators that filtrating is carried out concentrating under reduced pressure, isolate alcoholic solution; After ethanol is separated, the concentrate adding distil water is dissolved, lysate moves in the centrifuge tube; Centrifugally in centrifuge remove a small amount of water-fast impurity; Carefully draw supernatant with glue head dropper, be collected in the 100mL volumetric flask adding distil water standardize solution.
The optimum extraction process that obtains flavone in the Broussonetia papyrifera staminate inflorescence through experiment is that concentration of alcohol is 20%, and extracting temperature is 85 ℃, and solid-liquid ratio is 1:20g/mL, and extraction time is 3h.
2.2 Broussonetia papyrifera staminate inflorescence extractum preparation
With the flavone extractive of above-mentioned standardize solution, be rotated distillation 3h, make Broussonetia papyrifera staminate inflorescence extractum.
2.3 the preparation of Broussonetia papyrifera staminate inflorescence hard capsule
(1) selection of hard capsule diluent
The adjuvant that hard capsule preparation is commonly used has starch, sucrose, dextrin, soluble starch, lactose etc.Dextrin and starch are to use adjuvant more widely at present; The sucrose toughness can be made binding agent, and dextrin viscosity wants weak than sucrose viscosity, and relatively poor with the dissolubility of starch.Lactose is soluble in water, is good diluent, and the more good and stable in properties than sucrose character is the succedaneum and the no hygroscopicity of lactose, and is less to the influence that drug content is measured, and is good diluent.In addition, lactose also has the function of rectifying flavor concurrently.Soluble starch has improved the hygroscopicity of starch, and water-soluble, is a kind of new adjuvant.These article are selected lactose, sucrose and the soluble starch diluent as hard capsule, the three is mixed by different proportion with the staminate inflorescence extracting solution do the pelletize test.Result of the test is an extracting solution: lactose: sucrose: during soluble starch=1:1:1:3, the pelletize effect is best, in addition the double correctives of doing of lactose.
(2) selection of wetting agent
Wetting agent is modal to be the second alcohol and water, and their difference is the semi-polarity wetting agent for ethanol, and water is the polarity wetting agent; Alcoholic acid warp tension ratio water is little, when raw material contains extractum when more, uses the Different concentrations of alcohol water of granulating than making to granulate and suit; Because the water capacity is prone to make the granule hardening that makes; Be prone to caking, so these article select for use Different concentrations of alcohol solution to make an experiment experimental result as wetting agent: the uniform particles that the alcoholic solution of wetting agent selection 85% is made; Effective, and dry back is non-friable.
(3) manufacture method
Place baking oven to dry fully sucrose, lactose and soluble starch; Sucrose and lactose grind in mortar, with three kinds of adjuvants with Broussonetia papyrifera staminate inflorescence extractum: the ratio of sucrose: lactose: starch=1:1:1:3 takes by weighing, and gets an amount of 85% ethanol and is added to mixing in the extractum; With the standard pelletize of " that holds is agglomerating; that touches then looses ", afterwards granule is sieved, make its molecular sieve that passes 10 orders (sieve), do not pass the molecular sieve of 80 orders (No. five sieves).Place the baking oven of 85 ℃ of temperature to dry satisfactory granule afterwards.Treating to pack into after the particle drying cooling promptly can be made into Broussonetia papyrifera staminate inflorescence hard capsule in the Capsules, puts into shady and cool dry place then and preserves.
Claims (6)
1. the method for preparing of a Broussonetia papyrifera staminate inflorescence hard capsule; It may further comprise the steps: the first, and preparation Broussonetia papyrifera staminate inflorescence flavone extractive, its process is: take by weighing a certain amount of Broussonetia papyrifera staminate inflorescence powder sample; According to experiment of single factor and Orthogonal Experiment and Design; Change flavone extraction conditions adds the lixiviate that refluxes of 20%～30% alcoholic solution by solid-liquid ratio 1:20 in sample, change lixiviating solution over to cloth wet funnel and use vacuum pump to carry out sucking filtration and collect filtrating; Filtrating is gone in the evaporative flask, use Rotary Evaporators that filtrating is carried out concentrating under reduced pressure, isolate alcoholic solution; After ethanol is separated, the concentrate adding distil water is dissolved, lysate moves in the centrifuge tube, centrifugally in centrifuge removes water-fast impurity, draws supernatant with glue head dropper, is collected in the standardize solution measuring bottle adding distil water standardize solution; The second, Broussonetia papyrifera staminate inflorescence extractum preparation: with the flavone extractive of above-mentioned standardize solution, be rotated distillation 2.5h～3.5h, make Broussonetia papyrifera staminate inflorescence extractum; The 3rd, preparation Broussonetia papyrifera staminate inflorescence hard capsule, its process is: at first place baking oven to dry fully sucrose, lactose and soluble starch; Sucrose and lactose grind in mortar; With Broussonetia papyrifera staminate inflorescence extractum: the ratio of sucrose: lactose: starch=1:1:1:3 takes by weighing, and gets 80%～90% alcoholic solution and is added to mixing in the extractum, pelletize as wetting agent; Afterwards granule is sieved, make it pass 10 molecules of interest sieve, do not pass 80 molecules of interest sieve; The granule that will meet above requirement places the baking oven of 85 ℃ of temperature to dry, and is Broussonetia papyrifera staminate inflorescence hard capsule in the Capsules of treating to pack into after particle drying cools off, and puts into shady and cool dry place then and preserves.
2. the method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule according to claim 1 is characterized in that: in the first step, " taking by weighing a certain amount of Broussonetia papyrifera staminate inflorescence powder sample " is meant the Broussonetia papyrifera staminate inflorescence powder sample that takes by weighing 5g, 10g, 15g or 20g; " be collected in the standardize solution measuring bottle " and be meant in the standardize solution measuring bottle that is collected into 100 mL, 200 mL, 300 mL or 400 mL; The standardize solution measuring bottle at this place is corresponding with the Broussonetia papyrifera staminate inflorescence powder sample weight that takes by weighing respectively.
3. the method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule according to claim 1 is characterized in that: in the first step, " solid-liquid ratio 1:20 " is meant sample: alcoholic solution=1 g:20mL.
4. the method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule according to claim 1 is characterized in that: in the first step, the optimum extraction process of flavone is that concentration of alcohol is 20% in the Broussonetia papyrifera staminate inflorescence, and extracting temperature is 85 ℃, and the extraction time of backflow lixiviate is 3h.
5. the method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule according to claim 1 is characterized in that: in second step, and rotary distillation 3h.
6. the method for preparing of Broussonetia papyrifera staminate inflorescence hard capsule according to claim 1 is characterized in that: in the third step, get 85% alcoholic solution as wetting agent.
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| CN201210246079.7A CN102772490B (en) | 2012-07-17 | 2012-07-17 | Method for preparing paper mulberry staminate inflorescence hard capsule |
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| CN201210246079.7A CN102772490B (en) | 2012-07-17 | 2012-07-17 | Method for preparing paper mulberry staminate inflorescence hard capsule |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107304195A (en) * | 2016-04-21 | 2017-10-31 | 辽宁药联制药有限公司 | The screening of Flavonoid substances extraction process in century-old grass |
| CN107488507A (en) * | 2017-08-30 | 2017-12-19 | 北京市林业果树科学研究院 | A kind of Anti-oxidant agent containing Chinese Chestnut sequence extract and preparation method thereof |
| CN114053329A (en) * | 2021-12-30 | 2022-02-18 | 广东药科大学 | Application of broussonetia papyrifera in preparation of medicines or sunscreen cosmetics for preventing and treating ultraviolet injury |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101305758A (en) * | 2007-05-14 | 2008-11-19 | 刘尚文 | Broussonetia papyrifera leaves tea and its preparation method |
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2012
- 2012-07-17 CN CN201210246079.7A patent/CN102772490B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101305758A (en) * | 2007-05-14 | 2008-11-19 | 刘尚文 | Broussonetia papyrifera leaves tea and its preparation method |
Non-Patent Citations (3)
| Title |
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| 华栋等: "构树雄花序的营养成分", 《徐州师范大学学报(自然科学版)》 * |
| 张倩等: "雄构树花序化学成分研究", 《中药材》 * |
| 徐颖等: "构树不同部位总黄酮含量的季节性变化研究", 《现代中药研究与实践》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107304195A (en) * | 2016-04-21 | 2017-10-31 | 辽宁药联制药有限公司 | The screening of Flavonoid substances extraction process in century-old grass |
| CN107488507A (en) * | 2017-08-30 | 2017-12-19 | 北京市林业果树科学研究院 | A kind of Anti-oxidant agent containing Chinese Chestnut sequence extract and preparation method thereof |
| CN114053329A (en) * | 2021-12-30 | 2022-02-18 | 广东药科大学 | Application of broussonetia papyrifera in preparation of medicines or sunscreen cosmetics for preventing and treating ultraviolet injury |
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| CN102772490B (en) | 2014-12-10 |
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