CN102743349B - Small-volume puerarin freeze-dried powder injection and its preparation method and production device - Google Patents
Small-volume puerarin freeze-dried powder injection and its preparation method and production device Download PDFInfo
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- CN102743349B CN102743349B CN201210212364.7A CN201210212364A CN102743349B CN 102743349 B CN102743349 B CN 102743349B CN 201210212364 A CN201210212364 A CN 201210212364A CN 102743349 B CN102743349 B CN 102743349B
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Abstract
The invention belongs to the technical field of freeze-dried powder injection preparation and relates to a small-volume puerarin freeze-dried powder injection and its preparation method and production device. The small-volume puerarin freeze-dried powder injection is obtained by putting puerarin freeze-dried powder into a tube-type penicillin bottle having a volume of 7ml, wherein the small-volume puerarin freeze-dried powder injection contains 0.1 to 0.2g of puerarin. The preparation method comprises the following steps of taking prescription amounts of puerarin and auxiliary materials, adding injection water into the puerarin and the auxiliary materials, cooling to a temperature of 28 to 30 DEG C, preparing a strong solution, adding activated carbon into the strong solution, uniformly stirring, carrying out decarburization filtration by titanium rods, carrying out refined filtration, adding the residual amount of the injection water having a temperature of 28 to 30 DEG C into a liquid blending tank, carrying out filtration by titanium rods, carrying out refined filtration, mixing the filtrate, preparing the mixed filtrate into a dilute solution, keeping a temperature of 28 to 30 DEG C, loading the dilute solution into a tube-type penicillin bottle having a volume of 7ml, and carrying out freeze-drying, plug-pressing and lid-rolling. The preparation method and the production device reduce a packaging volume of the small-volume puerarin freeze-dried powder injection, effectively improve a yield, reduce energy consumption, reduce packaging and transportation costs, and greatly reduce freeze-drying evaporation energy consumption.
Description
Technical field
The invention belongs to freeze-dried powder preparing technical field, relate to a kind of small size puerarin freeze-drying powder pin, its preparation method and process units thereof.
Background technology
0.1g puerarin freeze-drying powder pin commercially available at present and 0.2g puerarin freeze-drying powder pin, 10ml is all used to be molded cillin bottle fill, thus it is large to there is inner container volume, thus the volume in freeze drying box shared by every bottle is just large, cause the shortcoming that every series-produced product yield is low, because the water solublity of puerarin itself is bad, thus need by a large amount of solvents just solubilized in preparation process, to make puerarin freeze-drying powder pin.Original preparing process does not have temperature to control, in dense timing temperature generally at 20 DEG C ~ 25 DEG C, therefore the 50 times of water adding principal agent are needed just can be dissolved, thus increase fill amount, in order to ensure the rate of sublimation of moisture in freeze-drying process, use 10ml to be molded cillin bottle fill, cause that the output often criticized reduces, the moisture multipotency consumption of lyophilizing increases, packaging and cost of transportation increase.
Summary of the invention
The object of this invention is to provide a kind of small size puerarin freeze-drying powder pin, its preparation method and process units thereof, the method makes the volume-diminished of puerarin freeze-drying powder pin, output rising, energy consumption reduce, and decreases packaging and cost of transportation.
Small size puerarin freeze-drying powder pin of the present invention is contained in by puerarin freeze-drying powder in 7ml control cillin bottle, and the puerarin content in puerarin freeze-drying powder pin is 0.1g or 0.2g.
Described 0.1g small size puerarin freeze-drying powder is contained in 7ml control cillin bottle, its washmarking position with lower volume for 3 ~ 3.5ml.
Described 0.2g small size puerarin freeze-drying powder is contained in 7ml control cillin bottle, its washmarking position with lower volume for 4 ~ 4.5ml.
The preparation method of small size puerarin freeze-drying powder pin of the present invention, comprises the steps:
(1) get puerarin and the adjuvant of recipe quantity, add water for injection and be down to 28 DEG C ~ 30 DEG C and make concentrated wiring liquid, be fully stirred to dissolve, add active carbon and stir, filter with the decarburization of titanium rod, fine straining;
(2) by the water for injection of residue amount of preparation, water temperature 28 DEG C ~ 30 DEG C, adds in Agitation Tank, after being filtered by titanium rod; Fine straining;
(3) step (2) gained filtrate and step (1) gained filtrate are mixed and made into rare dosing, are incubated 28 DEG C ~ 30 DEG C, fill is in 7ml control cillin bottle, and lyophilizing, tamponade, to roll lid obtained.
The device of the small size puerarin freeze-drying powder pin described in manufacture, the second Grandfos pump of the insulation dispensing canister connected by utilidor successively, conveying feed liquid, titanium rod filter, the second degerming filter element, aseptic insulation liquid storage tank, conveying the first Grandfos pump of feed liquid, the first degerming filter element, filling machine and freeze dryer form.
Research process:
One, for the character of puerarin dissolubility in water, select the water for injection of three kinds of different temperatures to dissolve, dissolve the injection water yield needed for 1g puerarin at different temperatures in table 1; After abundant stirring and dissolving, investigate the impact of its solution temperature on puerarin and adjuvant mixed solution stability, represent with puerarin content, the results are shown in Table 2.
Table 1 solution temperature and water for injection volume synopsis
| Solution temperature DEG C | Water for injection volume ml |
| 50℃ | 20ml |
| 40℃ | 25ml |
| 30℃ | 31.05ml |
On the impact of principal agent puerarin stability under table 2 different temperatures
As can be seen from Table 2, puerarin is 12 hours intensive amount stability in the aqueous solution of different temperatures, and the water for injection of 50 DEG C does not affect the stability of puerarin as can be seen here, in order to economize on resources, therefore adopts the water for injection of 28 DEG C ~ 30 DEG C.
Two, for the character of puerarin dissolubility in water, select the water for injection of three kinds of different temperatures to dissolve, dissolve the injection water yield needed for 2g puerarin at different temperatures in table 3.After abundant stirring and dissolving, investigate the impact of its solution temperature on puerarin and adjuvant mixed solution stability; The results are shown in Table 4.
Table 3 solution temperature and water for injection volume synopsis
| Solution temperature DEG C | Water for injection |
| 50℃ | 20ml |
| 40℃ | 30ml |
| 30℃ | 42.5ml |
On the impact of principal agent puerarin stability under table 4 different temperatures
As can be seen from Table 4, puerarin is 12 hours intensive amount stability in the aqueous solution of different temperatures, and the water for injection of 50 DEG C does not affect the stability of puerarin as can be seen here, in order to economize on resources, therefore adopts the water for injection of 28 DEG C ~ 30 DEG C.
Compared with prior art, the invention has the beneficial effects as follows:
Present invention decreases the packaging volume of puerarin freeze-drying powder pin, thus effectively increase output, reduce energy consumption, while reducing packaging, cost of transportation, greatly reduce lyophilizing evaporation energy consumption.
Accompanying drawing explanation
Fig. 1 is apparatus structure schematic diagram of the present invention;
Wherein: 1, be incubated dispensing canister; 2, titanium rod filter; 3, aseptic insulation liquid storage tank; 4, freeze dryer; 5, filling machine; 6, the first Grandfos pump; 7, the first degerming filter element; 8, the second degerming filter element; 9, the second Grandfos pump; 10, utilidor.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
The preparation method of 0.1g small size puerarin freeze-drying powder pin:
Its formula is as follows:
Water for injection is added in insulation dispensing canister, mannitol is added when being down to below 35 DEG C, stirring and dissolving, solution temperature is down to 28 ~ 30 DEG C, add puerarin, sodium bicarbonate, natrium carbonicum calcinatum successively again, after puerarin dissolves completely, add sodium sulfite, abundant stirring, feed temperature remains between 28 ~ 30 DEG C.Feed liquid molten clear after, sampling detects material liquid pH value and controls between 8.10 ~ 8.25 (pH standard 7.5 ~ 9.0), adds 0.1%(W/V) activated carbon decolorizing 30 minutes.
Open the second Grandfos pump titanium rod filter decarburization to filter, feed liquid is degerming by the second degerming filter element, and be transported in aseptic insulation liquid storage tank and store.Aseptic filtration is complete, is added by the water for injection of surplus in insulation dispensing canister, degerming by the second degerming filter element again after titanium rod filter, and is transported in aseptic insulation liquid storage tank.Open aseptic insulation liquid storage tank feed liquid circulating pump, feed liquid, through the first Grandfos pump, the first degerming filter element, by filling machine fill, by the fill of 3.1ml/ bottle in 7ml control cillin bottle, then by freeze dryer lyophilizing, through tamponade, rolls lid, and packaging is obtained.
Product temperature is down to-35 DEG C, maintain 1 hour, after again condensation tube temperature being down to-45 DEG C, set refrigerant temperature as-8 DEG C, maintain 15 hours, rise to 5 DEG C again, maintain 5 hours, finally setting refrigerant temperature is 50 DEG C, maintains 9 hours, the gas source switch input filtrated air of casing is opened, by " freeze dryer standard operating procedure " tamponade after final drying.
The device of the small size puerarin freeze-drying powder pin described in manufacture, the degerming filter element 7 of the first Grandfos pump 6, first of the second Grandfos pump 9 of the insulation dispensing canister 1 connected by utilidor 10 successively, conveying feed liquid, titanium rod filter 2, second degerming filter element 8, aseptic insulation liquid storage tank 3, conveying feed liquid, filling machine 5 and freeze dryer 4 form.Described insulation dispensing canister 1 model: F-1000L volume: 1000 liters.
Embodiment 2
The preparation method of 0.2g small size puerarin freeze-drying powder pin:
Water for injection is added in insulation dispensing canister, mannitol is added when being down to below 35 DEG C, stirring and dissolving, solution temperature is down to 28 ~ 30 DEG C, add puerarin, sodium bicarbonate, natrium carbonicum calcinatum successively again, after puerarin dissolves completely, add sodium sulfite, abundant stirring, feed temperature remains between 28 ~ 30 DEG C.Feed liquid molten clear after, sampling detects between material liquid pH 8.10 ~ 8.25 (pH standard 7.5 ~ 9.0), adds 0.1%(W/V) activated carbon decolorizing 30 minutes.
Open the second Grandfos pump titanium rod filter decarburization to filter, feed liquid is degerming by the second degerming filter element, and be transported in aseptic insulation liquid storage tank and store.Aseptic filtration is complete, is added by the water for injection of surplus in insulation dispensing canister, degerming by the second degerming filter element again after titanium rod filter, and is transported in aseptic insulation liquid storage tank.Open aseptic insulation liquid storage tank feed liquid circulating pump, feed liquid, through the first Grandfos pump, the first degerming filter element, by filling machine fill, by the fill of 4.2ml/ bottle in 7ml control cillin bottle, then by freeze dryer lyophilizing, through tamponade, rolls lid, and packaging is obtained.
Product temperature is down to-35 DEG C, maintain 1 hour, after again condensation tube temperature being down to-45 DEG C, set refrigerant temperature as-8 DEG C, maintain 15 hours, rise to 5 DEG C again, maintain 5 hours, finally setting refrigerant temperature is 50 DEG C, maintains 9 hours, the gas source switch input filtrated air of casing is opened, by " freeze dryer standard operating procedure " tamponade after final drying.
The device of the 0.2g small size puerarin freeze-drying powder pin described in manufacture and insulation dispensing canister model are as embodiment 1.
Claims (1)
1. a preparation method for small size puerarin freeze-drying powder pin, is characterized in that formula is as follows:
Puerarin 100g
Mannitol 100g
Sodium bicarbonate 10g
Natrium carbonicum calcinatum 23g
Sodium sulfite 8g
Water for injection adds to 3100ml,
Make 1000;
Water for injection is added in insulation dispensing canister, mannitol is added when being down to below 35 DEG C, stirring and dissolving, solution temperature is down to 28 ~ 30 DEG C, add puerarin, sodium bicarbonate, natrium carbonicum calcinatum successively again, after puerarin dissolves completely, add sodium sulfite, abundant stirring, feed temperature remains on 28 ~ 30 DEG C; Feed liquid molten clear after, sampling detects material liquid pH value and controls 8.10 ~ 8.25, adds the activated carbon decolorizing 30 minutes that w/v is 0.1%;
Open the second Grandfos pump titanium rod filter decarburization to filter, feed liquid is degerming by the second degerming filter element, and be transported in aseptic insulation liquid storage tank and store; Aseptic filtration is complete, is added by the water for injection of surplus in insulation dispensing canister, degerming by the second degerming filter element again after titanium rod filter, and is transported in aseptic insulation liquid storage tank; Open aseptic insulation liquid storage tank feed liquid circulating pump, feed liquid, through the first Grandfos pump, the first degerming filter element, by filling machine fill, by the fill of 3.1ml/ bottle in 7ml control cillin bottle, then by freeze dryer lyophilizing, through tamponade, rolls lid, and packaging is obtained;
Product temperature is down to-35 DEG C, maintain 1 hour, after again condensation tube temperature being down to-45 DEG C, set refrigerant temperature as-8 DEG C, maintain 15 hours, rise to 5 DEG C again, maintain 5 hours, finally setting refrigerant temperature is 50 DEG C, maintains 9 hours, the gas source switch input filtrated air of casing is opened, by " freeze dryer standard operating procedure " tamponade after final drying;
The device of the small size puerarin freeze-drying powder pin described in manufacture, the second Grandfos pump (9) of the insulation dispensing canister (1) connected by utilidor (10) successively, conveying feed liquid, titanium rod filter (2), the second degerming filter element (8), aseptic insulation liquid storage tank (3), conveying the first Grandfos pump (6) of feed liquid, the first degerming filter element (7), filling machine (5) and freeze dryer (4) form; Described insulation dispensing canister 1 model: F-1000L volume: 1000 liters.
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| CN102743349B true CN102743349B (en) | 2015-07-01 |
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| CN104510711A (en) * | 2013-09-30 | 2015-04-15 | 瑞阳制药有限公司 | Small-volume asarin freeze-dried powder injection, preparation method and producing apparatus thereof |
| CN106806349A (en) * | 2015-11-30 | 2017-06-09 | 湖南恒生制药股份有限公司 | Puerarin freeze-drying powder-injection and preparation method thereof |
| CN113143861B (en) * | 2021-06-15 | 2022-09-13 | 华北制药股份有限公司 | Puerarin composition for injection and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242217A (en) * | 1998-07-17 | 2000-01-26 | 烟台绿叶制药有限公司 | Traditional Chinese medicine compositions contg. pueraria root extract |
| CN101953803A (en) * | 2010-09-02 | 2011-01-26 | 天津市铭泰医药科技有限公司 | Preparation method of small-volume doxofylline freeze-dried powder injection as well as product and device thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242217A (en) * | 1998-07-17 | 2000-01-26 | 烟台绿叶制药有限公司 | Traditional Chinese medicine compositions contg. pueraria root extract |
| CN101953803A (en) * | 2010-09-02 | 2011-01-26 | 天津市铭泰医药科技有限公司 | Preparation method of small-volume doxofylline freeze-dried powder injection as well as product and device thereof |
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Denomination of invention: Small-volume puerarin freeze-dried powder injection and its preparation method and production device Effective date of registration: 20161027 Granted publication date: 20150701 Pledgee: Agricultural Bank of China, Limited by Share Ltd, Yiyuan county subbranch Pledgor: Reyoung Pharmaceutical Co., Ltd. Registration number: 2016990000912 |
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Address after: 256100 No. 6 Erlang Road, Yiyuan County, Zibo, Shandong Patentee after: Ruiyang Pharmaceutical Co., Ltd Address before: 256100 No. 6 Erlang Road, Yiyuan County, Zibo, Shandong Patentee before: REYOUNG PHARMACEUTICAL Co.,Ltd. |
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Date of cancellation: 20201228 Granted publication date: 20150701 Pledgee: Agricultural Bank of China Limited by Share Ltd. Yiyuan county subbranch Pledgor: REYOUNG PHARMACEUTICAL Co.,Ltd. Registration number: 2016990000912 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right |