CN101703484B - Preparation method of hexadecadrol sodium phosphate freeze-dried powder injection - Google Patents
Preparation method of hexadecadrol sodium phosphate freeze-dried powder injection Download PDFInfo
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- CN101703484B CN101703484B CN2009102503409A CN200910250340A CN101703484B CN 101703484 B CN101703484 B CN 101703484B CN 2009102503409 A CN2009102503409 A CN 2009102503409A CN 200910250340 A CN200910250340 A CN 200910250340A CN 101703484 B CN101703484 B CN 101703484B
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Abstract
The invention provides a preparation method of hexadecadrol sodium phosphate freeze-dried powder injection, which comprises the following steps: mannitol is dissolved, added with active carbon, boiled and filtered, added with the hexadecadrol sodium phosphate and prepared to a liquid medicine; the liquid medicine is treated by prefreezing, primary freeze drying and secondary freeze drying; and then hydraulic pressure adding stopper, rolling cap and packaging are carried out. The method has the advantages that the method improves the liquid medicine preparation and freeze-drying technology, does not affect the content of the hexadecadrol sodium phosphate, can increase the single batch output, simultaneously shortens the freeze-drying time, increases the product stability, saves the energy, increases the production and reduces the production cost.
Description
Technical field
The present invention relates to medical technical field, specifically, relate to a kind of method for preparing of dexamethasone sodium phosphate lyophilized injectable powder.
Background technology
Dexamethasone sodium phosphate is an adrenal cortex hormones drug; Be mainly used in anaphylaxis and autoimmune inflammation property disease; Be used for connective tissue disease, activeness rheumatism, rheumatoid arthritis, lupus erythematosus, serious bronchial asthma, serious dermatitis, ulcerative colitis, acute leukemia etc. more, also be used for the Comprehensive Treatment of some severe infections and poisoning, malignant lymphoma.The chemical name of dexamethasone sodium phosphate is 16 Alpha-Methyls-11 β, 17 α, and 21-trihydroxy-9 α-fuprednate-1,4-diene-3,20-diketone-21-organic phosphate disodium salt, molecular formula is C
22H
28FNa
2O
8P, molecular weight are 516.41.
The dexamethasone sodium phosphate lyophilized injectable powder is in dexamethasone sodium phosphate, to add the aseptic freeze-dried article that proper excipient is processed, and is the lyophilizing bulk or the powder of white or off-white color, and two kinds of specifications of 2mg and 5mg (by dexamethasone sodium phosphate) are arranged usually.Its production procedure is: lid-visual inspection-packing is rolled in medicinal liquid preparation-fill false add plug-lyophilization-tamponade.
At present, the method for preparing of dexamethasone sodium phosphate lyophilized injectable powder has following two kinds:
Method one:
(1) preparating liquid: lyophilized powder proppant and antioxidant are dissolved in leading in the water for injection of nitrogen of total amount of preparation 70%, and regulating pH is 8.0～8.4, adds dexamethasone sodium phosphate; And supply surplus with water for injection; Stirring and dissolving adds 0.5% (w/v) active carbon, stirring at room 30min; Filter carbon removal, subsequent use behind the reuse 0.22 μ m filtering with microporous membrane.
(2) lyophilization: get above-mentioned fine straining liquid, be sub-packed in the 10mL glass tube vial by every bottle of 5mL (2mg specification), glass tube vial places freezer dryer, in-45 ℃ of insulation 5h, carries out pre-freeze; The open cold condenser is regulated vacuum to 20Pa then, and the flaggy temperature that raises gradually is to-5 ℃; Insulation 10～12h; Continue 1h to 0 ℃ of intensification insulation 3h then, when products temperature and flaggy temperature near the time, continuation rising flaggy temperature also is incubated more than the 4h for 1h to 30 ℃; When products temperature and flaggy temperature once more near the time finish lyophilizing, tamponade is rolled lid, is packed.Total freeze-drying time is more than 25h.
Method two:
(1) preparating liquid: will claim that fixed lactose, dextran add in an amount of water for injection, and be stirred to dissolving fully, and add dexamethasone sodium phosphate; After the dissolving, add the active carbon of 0.3% (w/v) fully, boil 30min; Filter carbon removal, add the water for injection of full dose volume 50%, regulate pH to 7.5～8.5; Supply surplus with water for injection, be filtered to basin, process semi-finished product through germ tight filter.
(2) lyophilization: above-mentioned semi-finished product are sub-packed in the 7mL glass tube vial by every bottle of 2mL, and lid is rolled in lyophilizing, packing.More than total freeze-drying time 26h.
But; The shortcoming of above-mentioned two kinds of methods is: (1) is in the preparating liquid process; Owing to all add active carbon again after the dissolving at raw material and adjuvant; Therefore remove the endotoxic while at active carbon, also can adsorb a small amount of dexamethasone sodium phosphate, thereby make Determination of Dexamethasone Sodium Phosphate descend about 5.0%～8.0%; (2) when packing the medicinal liquid branch into glass tube vial, because the floor space of 7mL that selects for use usually or 10mL glass tube vial is bigger, when using identical freeze dryer, single batch of output is less, and production cost is high; (3) aqueous solution of dexamethasone sodium phosphate is than the poor stability of dry powder, because the dexamethasone sodium phosphate lyophilized injectable powder in process of production, need be dissolved into aqueous solution earlier; Therefore freeze-drying time is long more; Dexamethasone sodium phosphate is in that time of non-drying regime is long more, and product quality is more unstable, and existing method freeze-drying time surpasses 25h; And energy consumption is big, and production cost is high.
In order to address the above problem, a kind of dexamethasone sodium phosphate lyophilized injectable powder of the present invention has improved the operation and the freeze-dry process of preparating liquid, has shortened freeze-drying time, helps improving the quality of products and saving energy and reduce the cost.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing of dexamethasone sodium phosphate lyophilized injectable powder.
In order to realize the object of the invention, the method for preparing of dexamethasone sodium phosphate lyophilized injectable powder of the present invention comprises the steps:
1) preparating liquid: mannitol is dissolved in the water for injection, adds active carbon, boil 15～30min after, filter carbon removal; Add water for injection, dexamethasone sodium phosphate, it is dissolved fully; Regulating pH is 7.0～8.5, supplies surplus with water for injection then, makes that the concentration of dexamethasone sodium phosphate is 2～5g/L, and filtration sterilization is mixed with medicinal liquid;
2) pre-freeze: in advance the condenser temperature of freezer dryer is reduced to below-40 ℃, the medicinal liquid branch of step 1) is packed in the glass tube vial, put into freezer dryer; In 1～2h, regulate the flaggy temperature to below-35 ℃, freezing 2h;
3) primary drying: the vacuum of regulating freezer dryer is increased to 4～6 ℃ with the flaggy temperature in 1h to 20Pa, insulation 4～5h;
4) redrying: regulate vacuum at 10～20Pa, in 1h, the flaggy temperature is warming up to 14～16 ℃, insulation 2h; In 1h, continue then the flaggy temperature to be risen to 38～40 ℃, insulation 4～5h;
Wherein, the weight ratio of dexamethasone sodium phosphate and mannitol is 2～5: 20～80 in the step 1).The addition of said active carbon is for pressing cumulative volume 1.0～2.0g/L.
Step 2) glass tube vial described in is preferably the 2mL glass tube vial, every bottled 1mL (2～5mg specification) medicinal liquid.
Especially, lyophilization total time of the present invention is 16～19h.After lyophilizing finished, lid, packing are jumped a queue, rolled to hydraulic pressure.
The present invention passes through the operation of preparation medicinal liquid and the improvement of freeze drying process; Its beneficial effect has: in (1) injection production technology, guaranteeing under the product quality premise that adjuvant is selected for use few more good more; The method for preparing of dexamethasone sodium phosphate lyophilized injectable powder of the present invention; Only select for use a kind of adjuvant of mannitol to do freeze-dried excipient, dexamethasone sodium phosphate is shaped in freeze-drying process easily, can guarantee the quality of product again; (2) in the process of preparating liquid, after charcoal treatment, add dexamethasone sodium phosphate at mannitol solution again, avoided dexamethasone sodium phosphate to reduce problem because of the content that activated carbon adsorption causes; (3) preferably use the 2mL glass tube vial as a minute packaging container, it is compared with 7mL or 10mL glass tube vial, and when using identical freeze dryer, single batch of output can double, thereby has reduced production cost; (4) in freeze-drying process; Improve pre-freeze speed, can apace medicinal liquid have been freezed to below the eutectic point, shortened freeze-drying time simultaneously; With freeze-drying time from foreshortening to 16～19h more than the 25h; Thereby further improved the stability of dexamethasone sodium phosphate, saved energy consumption simultaneously, cut down the consumption of energy 26%～38%; Owing to shortened freeze-drying time, under the situation that does not increase the hardware input, can improve production production capacity 26%～38%, energy-saving and production-increase simultaneously.
The invention has the advantages that the method for preparing of dexamethasone sodium phosphate lyophilized injectable powder of the present invention does not influence Determination of Dexamethasone Sodium Phosphate; And can improve single batch of output, shorten freeze-drying time simultaneously, thereby improve product stability; And energy-saving and production-increase has reduced production cost.
The specific embodiment
Following examples are used for further specifying the present invention, but are not used for limiting the present invention.
Embodiment 1
Dexamethasone sodium phosphate 20g
Mannitol 800g
Water for injection is added to 10L
(1) preparating liquid: quantitatively take by weighing 800g mannitol, add 6L water for injection, be stirred to dissolving fully, add the active carbon of 2.0g/L by the full dose volume, boil 30min after, filter carbon removal; Add 2L water for injection, 20g dexamethasone sodium phosphate, it is dissolved fully, recording the medicinal liquid pH value is 8.12, adds water for injection to 10L, and the germ tight filter of warp 0.22 μ m microporous filter membrane is filtered to basin, is mixed with medicinal liquid, and is subsequent use;
(2) lyophilization: the condenser temperature of freezer dryer (FCM50D type) is reduced to below-40 ℃ in advance; Above-mentioned medicinal liquid is sub-packed in the 2mL glass tube vial by every bottle of 1mL (2mg specification); Put into lyophilization mechanical goods chamber flaggy; In 1h, the flaggy temperature is reduced to below-35 ℃, keeps low temperature state 2h, carry out pre-freeze; The open vacuum pump, the vacuum of regulating freezer dryer rises to 5 ℃ with the flaggy temperature in 1h to 20Pa, and insulation 5h carries out primary drying; Control vacuum then at 10～20Pa, in 1h, the flaggy temperature is risen to 15 ℃, insulation 2h, and then to continue intensification 1h be 39 ℃ to the flaggy temperature, insulation 5h.(lyophilizing total time is 18h).
(3) after lyophilizing finishes, carry out hydraulic pressure and jump a queue, roll lid, packing.
The full testing result of product is as shown in table 1.
The full testing result of table 1 product
| Test item | Standard code | Assay |
| Character | White or off-white color dried frozen aquatic products | Up to specification |
| Differentiate | Drug standard YBH24032005 | Up to specification |
| Content | Should be 90.0～110.0% of labelled amount | 99.26％ |
| PH value | 7.0～8.5 | 8.12 |
| Loss on drying | ≤5.0％ | 1.1％ |
| Visible foreign matters | Drug standard YBH24032005 | Up to specification |
| Particulate matter | Drug standard YBH24032005 | Up to specification |
| Aseptic | Drug standard YBH24032005 | Up to specification |
| Thermal source | Drug standard YBH24032005 | Up to specification |
| Clarity of solution | Drug standard YBH24032005 | Up to specification |
Embodiment 2
Dexamethasone sodium phosphate 50g
Mannitol 200g
Water for injection is added to 10L
(1) preparating liquid: quantitatively take by weighing 200g mannitol, add 3L water for injection, be stirred to dissolving fully, add the active carbon of 1.0g/L by the full dose volume, boil 15min after, filter carbon removal; Add 5L water for injection, the 50g dexamethasone sodium phosphate dissolves it fully, and recording the medicinal liquid pH value is 8.02, adds water for injection to 10L, and the germ tight filter of warp 0.22 μ m microporous filter membrane is filtered to basin, is mixed with medicinal liquid, and is subsequent use;
(2) lyophilization: the condenser temperature of freezer dryer (FCM50D type) is reduced to below-40 ℃ in advance; Above-mentioned medicinal liquid is sub-packed in the 2mL glass tube vial by every bottle of 1mL (5mg specification); Put into lyophilization mechanical goods chamber flaggy; In 1h, the flaggy temperature is reduced to below-35 ℃, keeps low temperature state 2h, carry out pre-freeze; The open vacuum pump, the vacuum of regulating freezer dryer rises to 5 ℃ with the flaggy temperature in 1h to 20Pa, and insulation 4h carries out primary drying; Control vacuum then at 10～20Pa, in 1h, the flaggy temperature is risen to 15 ℃, insulation 2h, and then to continue intensification 1h be 38 ℃ to the flaggy temperature, insulation 4h.(lyophilizing total time is 16h).
(3) after lyophilizing finishes, carry out hydraulic pressure and jump a queue, roll lid, packing.
The full testing result of product is as shown in table 2.
The full testing result of table 2 product
| Test item | Standard code | Assay |
| Character | White or off-white color dried frozen aquatic products | Up to specification |
| Differentiate | Drug standard YBH24032005 | Up to specification |
| Content | Should be 90.0～110.0% of labelled amount | 99.40％ |
| PH value | 7.0～8.5 | 8.02 |
| Loss on drying | ≤5.0％ | 0.9％ |
| Visible foreign matters | Drug standard YBH24032005 | Up to specification |
| Particulate matter | Drug standard YBH24032005 | Up to specification |
| Aseptic | Drug standard YBH24032005 | Up to specification |
| Thermal source | Drug standard YBH24032005 | Up to specification |
| Clarity of solution | Drug standard YBH24032005 | Up to specification |
Embodiment 3
Dexamethasone sodium phosphate 20g
Mannitol 600g
Water for injection is added to 10L
(1) preparating liquid: quantitatively take by weighing 600g mannitol, add 5L water for injection, be stirred to dissolving fully, add the active carbon of 2.0g/L by the full dose volume, boil 20min after, filter carbon removal; Add 3L water for injection, 50g dexamethasone sodium phosphate, it is dissolved fully, recording the medicinal liquid pH value is 8.06, adds water for injection to 10L, and the germ tight filter of warp 0.22 μ m microporous filter membrane is filtered to basin, is mixed with medicinal liquid, and is subsequent use;
(2) lyophilization: the condenser temperature of freezer dryer (FCM50D type) is reduced to below-40 ℃ in advance; Above-mentioned medicinal liquid is sub-packed in the 2mL glass tube vial by every bottle of 1mL (2mg specification); Put into lyophilization mechanical goods chamber flaggy; In 1h, the flaggy temperature is reduced to below-35 ℃, keeps low temperature state 2h, carry out pre-freeze; The open vacuum pump, the vacuum of regulating freezer dryer rises to 5 ℃ with the flaggy temperature in 1h to 20Pa, and insulation 4h carries out primary drying; Control vacuum then at 10～20Pa, in 1h, the flaggy temperature is risen to 15 ℃, insulation 2h, and then to continue intensification 1h be 39 ℃ to the flaggy temperature, insulation 5h.(lyophilizing total time is 17h).
(3) after lyophilizing finishes, carry out hydraulic pressure and jump a queue, roll lid, packing.
The full testing result of product is as shown in table 3.
The full testing result of table 3 product
| Test item | Standard code | Assay |
| Character | White or off-white color dried frozen aquatic products | Up to specification |
| Differentiate | Drug standard YBH24032005 | Up to specification |
| Content | Should be 90.0～110.0% of labelled amount | 99.42％ |
| PH value | 7.0～8.5 | 8.06 |
| Loss on drying | ≤5.0％ | 0.8％ |
| Visible foreign matters | Drug standard YBH24032005 | Up to specification |
| Particulate matter | Drug standard YBH24032005 | Up to specification |
| Aseptic | Drug standard YBH24032005 | Up to specification |
| Thermal source | Drug standard YBH24032005 | Up to specification |
| Clarity of solution | Drug standard YBH24032005 | Up to specification |
Below further specify the present invention through stability test.
Experimental example 1 stable accelerated test
Respectively prepare 1 batch according to the method for embodiment 1,2 and 3 and prepare 3 batches of dexamethasone sodium phosphate lyophilized injectable powders altogether; Carry out accelerated test; The dexamethasone sodium phosphate lyophilized formulations that is about to process is put in 40 ± 2 ℃ the calorstat; Respectively at 0,1,3,6 month inspection character, pH value, loss on drying, four investigation projects of content, detect according to drug standard WS1-(X-016) 2006Z, the result is as shown in table 4.
The stable accelerated test result of table 4
Can find out that from table 4 each item index does not have significant change, all meet the regulation of the national drug standards, explain that the stability of the dexamethasone sodium phosphate lyophilized injectable powder that adopts the inventive method preparation is better.And, the 6th the end of month sample changes of contents be respectively 1.36%, 1.32%, 1.30%, average out to (1.33 ± 0.03) %, RSD=2.29 has further verified the reliability of process conditions of the present invention.
The product stability controlled trial of experimental example 2 the inventive method and existing method
Respectively prepare 3 batches of lyophilized injectable powders (feeding intake) according to existing method one, method two and embodiment 1 by 100% content; And the sample of processing placed 40 ± 2 ℃ calorstat; Carry out accelerated test, respectively at 0,6 month character of taking a sample to check, pH value, loss on drying, content four indices.Wherein pH value, loss on drying, content are the meansigma methods of 3 lot sample article, and the result sees table 5.
The stable controlled trial result of table 5
Can find out that from table 5 though the sample that makes by existing method meets national drug standards content, the loss on drying index changes obviously, processes product from being dosed into, content reduces above 6.0%; Loss on drying then reaches more than 3.0%, and after 6 months accelerated tests, content reduces above 8.0%; Loss on drying then reaches more than 4.0%, and adopts the sample stability of the inventive method preparation better, and content, loss on drying index change little; Process product from being dosed into, the content reduction is no more than 1.0%, and loss on drying is then less than 1.0%; After 6 months accelerated tests, the content reduction is no more than 2.0%, and loss on drying is then less than 2.0%.
Though; Through generality explanation, the specific embodiment and stability test the present invention has been done detailed description in the preceding text; But should be pointed out that for those skilled in the art, under the prerequisite that does not break away from know-why of the present invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (4)
1. the method for preparing of a dexamethasone sodium phosphate lyophilized injectable powder is characterized in that, comprises the steps:
1) preparating liquid: mannitol is dissolved in the water for injection, adds active carbon, boil 15～30min after, filter carbon removal; Add water for injection, dexamethasone sodium phosphate, it is dissolved fully; Regulate pH to 7.0～8.5, supply surplus with water for injection then, filtration sterilization is mixed with the semi-finished product medicinal liquid; The weight ratio of said dexamethasone sodium phosphate and mannitol is 2～5: 20～80;
2) pre-freeze: in advance condenser temperature is fallen below-40 ℃, the medicinal liquid branch of step 1) is packed in the glass tube vial, put into freezer dryer; In 1～2h, reduce the flaggy temperature to below-35 ℃, freezing 2h;
3) primary freeze drying: open vacuum pump, the vacuum of regulating freezer dryer rise to 4～6 ℃ with the flaggy temperature in the 1h below 20Pa, insulation 4～5h;
4) secondary freeze drying: keep vacuum at 10～20Pa, in the 1h flaggy temperature is risen to 14～16 ℃, insulation 2h; In 1h, continuing to be warming up to the flaggy temperature then is 38～40 ℃, insulation 4～5h.
2. method for preparing according to claim 1 is characterized in that, the addition of active carbon described in the step 1) is for pressing cumulative volume 1.0～2.0g/L.
3. method for preparing according to claim 1 is characterized in that, cryodesiccated total time is 16～19h.
4. method for preparing according to claim 1 is characterized in that step 2) described in glass tube vial be the 2mL glass tube vial, every bottled 1mL.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102309455A (en) * | 2010-07-02 | 2012-01-11 | 天津金耀集团有限公司 | Dexamethasone sodium phosphate powder injection and production method thereof |
| CN102743396B (en) * | 2011-04-22 | 2015-04-08 | 天津金耀集团有限公司 | Cortical hormone alkali metal phosphate composition |
| CN102293757B (en) * | 2011-08-30 | 2013-05-01 | 海南良方医药有限公司 | Dexamethasone Sodium Phosphate freeze-dried powder injection and preparation method thereof |
| CN105476965A (en) * | 2014-09-18 | 2016-04-13 | 蚌埠丰原涂山制药有限公司 | Method for preparing betamethasone sodium phosphate freeze-dried powder injection |
| CN104490796B (en) * | 2014-12-19 | 2017-07-04 | 成都天台山制药有限公司 | Injection dexamethasone sodium phosphate pharmaceutical composition and preparation method |
| CN105997897B (en) * | 2016-06-15 | 2018-04-17 | 马鞍山丰原制药有限公司 | A kind of amikacin sulfate lyophilized formulations and preparation method thereof |
| CN114198987A (en) * | 2021-11-11 | 2022-03-18 | 陕西孙思邈高新制药有限公司 | Freeze-drying process for traditional Chinese medicine standard decoction |
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