CN104856965A - Freeze-drying method of thymosin for injection - Google Patents
Freeze-drying method of thymosin for injection Download PDFInfo
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- CN104856965A CN104856965A CN201510288309.XA CN201510288309A CN104856965A CN 104856965 A CN104856965 A CN 104856965A CN 201510288309 A CN201510288309 A CN 201510288309A CN 104856965 A CN104856965 A CN 104856965A
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Abstract
The invention provides a freeze-drying method of thymosin for injection. The freeze-drying method comprises the following steps: cooling a thymosin solution sample to a first temperature which is less than or equal to minus 35 DEG C; under the condition of the first temperature, pre-freezing the thymosin solution sample under a vacuum condition; after the vacuum degree is less than 500ubar, heating the pre-frozen thymosin solution sample to a second temperature which is higher than minus 15 DEG C; cooling the thymosin solution sample from the second temperature to a third temperature which is not higher than minus 40 DEG C; heating the thymosin solution sample from the third temperature to a fourth temperature which is not less than 40 DEG C, and performing heat preservation under the condition of the fourth temperature so as to obtain a thymosin sample for injection. Compared with the prior art, the thymosin sample, obtained according to the freeze-drying method disclosed by the invention, for the injection has better redissolution, the average redissolution time in an embodiment I is 3S, and the average redissolution time under the shake-up condition is 2S.
Description
Technical field
The present invention relates to technical field of pharmaceuticals, particularly relate to a kind of freeze drying process of injection thymosin.
Background technology
Thymosin has another name called thymosin or thymic factor, be less than the 5000 daltonian polypeptide with physiologically active, the Thymosin alpha 1 (T α 1) that thymosin main active is made up of 28 aminoacid by the molecular weight extracted in health pig or calf thymus tissue.
Thymosin is used for the treatment of various constitutional or Secondary cases T cell defect disease clinically, some autoimmune disease, the auxiliary treatment of the disease that various cellular immune function is low and tumor, specifically comprises various hepatitis gravis, chronic active hepatitis, chronic persistent hepatitis and liver cirrhosis etc.; Herpes zoster, genital herpes, condyloma acuminatum etc.; 3. bronchitis, bronchial asthma, pulmonary tuberculosis, prevention upper respiratory tract infection etc.; Various malignant tumor early stage and chemotherapy, radiotherapy is share and is used; Lupus erythematosus, rheumatic and atrophic diseases, ankylosing spondylitis, Guillain Barre syndrome etc.; Aplastic anemia, leukemia, thrombocytopenia etc.; 7. viral keratitis, viral conjunctivitis, allergic rhinitis etc.; Senile senilism, menopausal syndrome etc.; Multiple furuncle and phyma and skin of face acne etc., psoriasis, lichen planus, squamous cell carcinoma and epithelium seborrheic keratosis etc.; Children with congenital immunodeficiency symptoms etc.
Existing thymosin administering mode comprises subcutaneous or intramuscular injection and oral.Injection thymosin is obtained by freeze-dried thymus peptide solution usually, and in prior art, injection thymosin freeze-dry process comprises: push in vacuum freeze drier by the glass bottle being loaded with medicinal liquid; Products temperature is down to less than-40 DEG C and starts evacuation, pre-freeze is about 240min; Treat that low vacuum is in 150ubar, rise to 40 DEG C with the speed of 3 DEG C/h from less than-40 DEG C, the cycle is about 1800min; About 400min is incubated at 40 DEG C; Close vacuum pump, stop vacuum, tamponade, outlet.The injection thymosin finished product solubility that this freeze-dry process obtains is poor, and the average redissolution time that the lyophilizing sample of 20mg adds 2mL water for injection is 72s, and the redissolution time shaken up under condition is 48s.
Summary of the invention
The object of the present invention is to provide a kind of freeze drying process of injection thymosin, the injection thymosin finished product redissolution performance that method lyophilizing provided by the invention obtains is good.
The invention provides a kind of freeze drying process of injection thymosin, comprise the following steps:
By greenhouse cooling to the first temperature of thymus peptide solution sample, described first temperature≤-35 DEG C;
Under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum;
Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C;
Again the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature, described 3rd temperature is not higher than-40 DEG C;
Again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.
Preferably, the time of described pre-freeze is 120min ~ 180min.
Preferably, the vacuum of described pre-freeze is 50 ~ 150ubar.
Preferably, the heating rate being warming up to the second temperature described in is 3 DEG C/h ~ 7 DEG C/h.
Preferably, described second temperature is-15 DEG C ~ 0 DEG C.
Preferably, the time that described second temperature is down to the 3rd temperature is preferably 300min ~ 600min.
Preferably, described 3rd temperature is-50 DEG C ~-40 DEG C.
Preferably, described 3rd temperature is 800 ~ 1000min to the time of the 4th temperature.
Preferably, described 4th temperature is 40 DEG C ~ 50 DEG C.
Preferably, the time of described insulation is 120 DEG C ~ 180 DEG C.
The invention provides a kind of freeze drying process of injection thymosin, comprise the following steps: by greenhouse cooling to the first temperature of thymus peptide solution sample, described first temperature≤-35 DEG C; Under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum; Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C; Again the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature, described 3rd temperature is not higher than-40 DEG C; Again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.Compared with prior art, the injection thymosin sample that method provided by the invention obtains has good solubility, the experimental result of the embodiment of the present invention shows, the average redissolution time under the condition of not shaking of the injection thymosin sample that the present invention obtains is 3s, and under shaking up condition, the average redissolution time is 2s.
And the injection thymosin sample n.s atrophy phenomenon that method provided by the invention obtains and cellular sample occur, ensure that the quality of product in effect duration.Method provided by the invention makes the medication of injection thymosin safer, and suitability for industrialized is produced in enormous quantities.
Detailed description of the invention
The invention provides a kind of freeze drying process of injection thymosin, comprise the following steps:
By greenhouse cooling to the first temperature of thymus peptide solution sample, described first temperature≤-35 DEG C;
Under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum;
Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C;
Again the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature, described 3rd temperature is not higher than-40 DEG C;
Again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.
Compared with prior art, the injection thymosin sample that method provided by the invention obtains has good solubility.And the injection thymosin sample n.s atrophy phenomenon that method provided by the invention obtains and cellular sample occur, ensure that the quality of product in effect duration.Method provided by the invention makes the medication of injection thymosin safer, and suitability for industrialized is produced in enormous quantities.
The temperature of thymus peptide solution sample is down to the first temperature by the present invention, described first temperature≤-35 DEG C.In an embodiment of the present invention, specifically in vacuum freeze drier, lyophilizing can be carried out to thymus peptide solution sample, preparation injection thymosin finished product.In the present invention, described first temperature is preferably-50 DEG C ~-35 DEG C, is more preferably-45 DEG C ~-40 DEG C.In the present invention, the mass concentration of described thymus peptide solution is preferably 5mg/mL ~ 20mg/mL, is more preferably 8mg/mL ~ 15mg/mL, most preferably is 10mg/mL ~ 15mg/mL.The source of the present invention to described thymus peptide solution does not have special restriction, adopts thymus peptide solution well known to those skilled in the art.In the present invention, the rate of temperature fall being cooled to the first temperature described in is preferably 13 ~ 17 DEG C/h.
After being cooled to the first temperature, the present invention under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum.In an embodiment of the present invention, after being cooled to the first temperature, specifically can opening vacuum pump and start evacuation, carry out pre-freeze.In the present invention, the vacuum of described pre-freeze is preferably 800ubar; The time of described pre-freeze is preferably 120min ~ 180min, is more preferably 135min ~ 165min, most preferably is 145min ~ 155min.In an embodiment of the present invention, in the process of pre-freeze, preferably continue cooling, until pre-freeze process terminates with above-mentioned rate of temperature fall.
Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C.Thymus peptide solution sample after pre-freeze, preferably when vacuum is down to 200ubar ~ 500ubar, is warming up to the second temperature, is more preferably 300ubar ~ 450ubar, is more preferably 350ubar ~ 400ubar by the present invention.In the present invention, described second temperature is preferably-15 DEG C ~ 0 DEG C, is more preferably-10 DEG C ~-5 DEG C; The described heating rate being warming up to the second temperature is preferably 3 DEG C/h ~ 7 DEG C/h, is more preferably 4 DEG C/h ~ 6 DEG C/h, most preferably is 5 DEG C/h.In the present invention, described in be warming up to the second temperature time be preferably 500min ~ 700min, be more preferably 550min ~ 650min, most preferably be 600min.
After being warming up to the second temperature, the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature by the present invention again, and described 3rd temperature is not higher than-40 DEG C.In the present invention, described 3rd temperature is preferably-50 DEG C ~-40 DEG C, is more preferably-48 DEG C ~-42 DEG C, most preferably is-45 DEG C; Described second greenhouse cooling is preferably 300min ~ 600min to the time of the 3rd temperature, is more preferably 320min ~ 500min, most preferably is 350min ~ 400min.In the present invention, described second greenhouse cooling is in the process of the 3rd temperature, and vacuum is preferably less than 800ubar.
After being cooled to the 3rd temperature, the present invention again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.In the present invention, described 3rd temperature is in the process of the 4th temperature, and vacuum is preferably less than 200ubar.In the present invention, described 4th temperature is preferably 40 DEG C ~ 50 DEG C, is more preferably 42 DEG C ~ 48 DEG C, most preferably is 45 DEG C; Described 3rd temperature is preferably 600 ~ 800min to the time of the 4th temperature.In the present invention, the time of described insulation is preferably 120min ~ 180min, is more preferably 135min ~ 165min, most preferably is 140min ~ 150min; The vacuum of described insulation is preferably 50 ~ 150ubar.
The invention provides a kind of freeze drying process of injection thymosin, comprise the following steps: by greenhouse cooling to the first temperature of thymus peptide solution sample, described first temperature≤-35 DEG C; Under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum; Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C; Again the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature, described 3rd temperature is not higher than-40 DEG C; Again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.Compared with prior art, the injection thymosin sample that method provided by the invention obtains has good solubility, the experimental result of the embodiment of the present invention shows, the average redissolution time under the condition of not shaking of the injection thymosin sample that the present invention obtains is 3s, and under shaking up condition, the average redissolution time is 2s.
And the injection thymosin sample n.s atrophy phenomenon that method provided by the invention obtains and cellular sample occur, ensure that the quality of product in effect duration.Method provided by the invention makes the medication of injection thymosin safer, and suitability for industrialized is produced in enormous quantities.
In order to further illustrate the present invention, being described in detail below in conjunction with the freeze drying process of embodiment to injection thymosin provided by the invention, but they can not being interpreted as limiting the scope of the present invention.
Embodiment 1
Be the thymus peptide solution fill 1000 of 10mg/mL by the concentration prepared, loading amount is 2.0mL, half tamponade;
Push in vacuum freeze drier by the glass bottle filling medicinal liquid, products temperature is down to-35 DEG C, the vacuum starting evacuation is less than 800ubar, pre-freeze 120min;
Until low vacuum after 500ubar, with the programming rate of 3 DEG C/h, products temperature is risen to-15 DEG C from-35 DEG C, the cycle is about 350min;
Again products temperature is down to-40 DEG C, the cooling used time is about 350min;
Finally products temperature is warming up to 40 DEG C, under the condition of 40 DEG C, is incubated 120min;
After being incubated, close vacuum pump, stop vacuum tamponade, outlet, obtain injection thymosin finished product.
The present invention detects the quality of the injection thymosin finished product obtained, observe that sample has the ratio of atrophy, sample appearance has cellular ratio, in sample, add the average redissolution time that the average redissolution time of 2mL water for injection and injection 2mL water for injection shakes up, result is as shown in table 1, and table 1 is the experimental result that the embodiment of the present invention and comparative example obtain.
Embodiment 2
Be the thymus peptide solution fill 1000 of 10mg/mL by the concentration prepared, loading amount is 2.0mL, half tamponade;
Push in vacuum freeze drier by the glass bottle filling medicinal liquid, products temperature is down to-35 DEG C, the vacuum starting evacuation is less than 800ubar, pre-freeze 180min;
Until low vacuum after 500ubar, with the programming rate of 7 DEG C/h, products temperature is risen to-15 DEG C from-35 DEG C, the cycle is about 172min;
Again products temperature is down to-40 DEG C, the cooling used time is about 500min;
Finally products temperature is warming up to 45 DEG C, under the condition of 45 DEG C, is incubated 150min;
After being incubated, close vacuum pump, stop vacuum tamponade, outlet, obtain injection thymosin finished product.
The present invention detects the quality of the injection thymosin finished product obtained, observe that sample has the ratio of atrophy, sample appearance has cellular ratio, in sample, add the average redissolution time that the average redissolution time of 2mL water for injection and injection 2mL water for injection shakes up, result is as shown in table 1, and table 1 is the experimental result that the embodiment of the present invention and comparative example obtain.
Embodiment 3
Be the thymus peptide solution fill 1000 of 10mg/mL by the concentration prepared, loading amount is 2.0mL, half tamponade;
The glass bottle filling medicinal liquid is pushed in vacuum freeze drier, products temperature is down to-35 DEG C, start evacuation and be less than 800ubar, pre-freeze 150min;
Until low vacuum after 500ubar, with the programming rate of 5 DEG C/h, products temperature is risen to-15 DEG C from-35 DEG C, the cycle is about 240min;
Again products temperature is down to-40 DEG C, the cooling used time is about 600min;
Finally products temperature is warming up to 42 DEG C, under the condition of 45 DEG C, is incubated 180min;
After being incubated, close vacuum pump, stop vacuum tamponade, outlet, obtain injection thymosin finished product.
The present invention detects the quality of the injection thymosin finished product obtained, observe that sample has the ratio of atrophy, sample appearance has cellular ratio, in sample, add the average redissolution time that the average redissolution time of 2mL water for injection and injection 2mL water for injection shakes up, result is as shown in table 1, and table 1 is the experimental result that the embodiment of the present invention and comparative example obtain.
Comparative example
Be the thymus peptide solution fill 1000 of 10mg/mL by the concentration prepared, loading amount is 2.0mL, half tamponade;
Push in vacuum freeze drier by the glass bottle being loaded with medicinal liquid, products temperature is down to less than-40 DEG C, start evacuation, pre-freeze is about 240min;
Treat that low vacuum is in 150ubar, rise to 40 DEG C with the programming rate of 3 DEG C/h from less than-40 DEG C, the cycle is about 1800min;
Be incubated about 400min at 40 DEG C, close vacuum pump after insulation, stop vacuum, tamponade, outlet, obtain injection thymosin finished product.
The present invention detects the quality of the injection thymosin finished product obtained, observe that sample has the ratio of atrophy, sample appearance has cellular ratio, in sample, add the average redissolution time that the average redissolution time of 2mL water for injection and injection 2mL water for injection shakes up, result is as shown in table 1, and table 1 is the experimental result that the embodiment of the present invention and comparative example obtain.
The experimental result that table 1 embodiment of the present invention and comparative example obtain
| Inspection item | Comparative example | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Sample number after lyophilizing | 1000 | 1000 | 1000 | 1000 |
| There is the sample size of atrophy | 72 | 0 | 0 | 0 |
| Outward appearance has cellular sample size | 421 | 0 | 0 | 0 |
| Average redissolution time (second) | 72 | 3 | 8 | 5 |
| Shake up the average redissolution time under condition | 48 | 2 | 5 | 3 |
As can be seen from Table 1, the injection thymosin finished product that method provided by the invention obtains is without atrophy, without cellular sample, and on average the redissolution time reduces greatly.
As can be seen from the above embodiments, the invention provides a kind of freeze drying process of injection thymosin, comprise the following steps: by greenhouse cooling to the first temperature of thymus peptide solution sample, described first temperature≤-35 DEG C; Under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum; Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C; Again the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature, described 3rd temperature is not higher than-40 DEG C; Again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.Compared with prior art, the injection thymosin sample that method provided by the invention obtains has good solubility, and in the injection thymosin finished product obtained, n.s atrophy phenomenon and cellular sample occur, ensure that the quality of product in effect duration.Method provided by the invention makes the medication of injection thymosin safer, and suitability for industrialized is produced in enormous quantities.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a freeze drying process for injection thymosin, comprises the following steps:
By greenhouse cooling to the first temperature of thymus peptide solution sample, described first temperature≤-35 DEG C;
Under the condition of described first temperature, by thymus peptide solution sample pre-freeze under vacuum;
Until low vacuum after 500ubar, the thymus peptide solution sample after pre-freeze is warming up to the second temperature, described second temperature is higher than-15 DEG C;
Again the temperature of thymus peptide solution sample is down to the 3rd temperature by described second temperature, described 3rd temperature is not higher than-40 DEG C;
Again by thymus peptide solution sample by described 3rd temperature to the 4th temperature, be incubated under the condition of the 4th temperature, obtain injection thymosin sample, described 4th temperature is not less than 40 DEG C.
2. freeze drying process according to claim 1, is characterized in that, the time of described pre-freeze is 120min ~ 180min.
3. freeze drying process according to claim 1, is characterized in that, the vacuum of described pre-freeze is 50 ~ 150ubar.
4. freeze drying process according to claim 1, is characterized in that, described in be warming up to the second temperature heating rate be 3 DEG C/h ~ 7 DEG C/h.
5. the freeze drying process according to claim 1 or 4, is characterized in that, described second temperature is-15 DEG C ~ 0 DEG C.
6. freeze drying process according to claim 1, is characterized in that, the time that described second temperature is down to the 3rd temperature is preferably 300min ~ 600min.
7. the freeze drying process according to claim 1 or 6, is characterized in that, described 3rd temperature is-50 DEG C ~-40 DEG C.
8. freeze drying process according to claim 1, is characterized in that, described 3rd temperature is 800 ~ 1000min to the time of the 4th temperature.
9. freeze drying process according to claim 1, is characterized in that, described 4th temperature is 40 DEG C ~ 50 DEG C.
10. the freeze drying process according to claim 1,8 or 9, is characterized in that, the time of described insulation is 120 DEG C ~ 180 DEG C.
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