CN102875574A - Crystal form of ceftriaxone sodium and preparation method for crystal form - Google Patents
Crystal form of ceftriaxone sodium and preparation method for crystal form Download PDFInfo
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Abstract
The invention discloses a novel crystal form of ceftriaxone sodium. The content of the novel crystal form is over 94 percent, and the novel crystal form is high in stability and accords with the medicinal standard. The invention also discloses a preparation method for the novel crystal form. By the method, a seed crystal is not required to be added, the preparation method is simple in operation, the yield is over 84 percent, and the novel crystal form is suitable for industrial production.
Description
Technical field
The invention belongs to medical technical field, relate to crystal formation of a kind of medicine and preparation method thereof, specifically finger spore Qusong sodium crystal and preparation method thereof.
Background technology
Ceftriaxone sodium belongs to third generation cephalosporin for injections class medicine, researched and developed by Switzerland Roche Holding Ag, chemical name is (6R, 7R)-7-[[(2-amino-4-thiazolyl) (methoxyimino) acetyl] amino]-8-oxo-3-[[(1,2,5,6-tetrahydrochysene-2 methyl-5,6-dioxo-1,2,4-triazine-3-yl) sulfo-] methyl]-5-sulfo--1-azabicyclo [4.2.0] oct-2-ene-three times of semihydrates of 2-carboxylic acid disodium salt, its structural formula is as follows:
Ceftriaxone sodium is semisynthetic cynnematin, and the synthetic performance anti-microbial effect by the anti-bacteria cell walls all has powerful anti-microbial activity to most of gram-positive microorganisms and Gram-negative bacteria.Be mainly used in the severe infections due to the responsive gram-positive cocci of responsive gram negative bacillus and part, because of its anti-microbial effect strong, long half time, curative effect is affirmed, clinical respiratory tract infection, septicemia, abdominal cavity infection, pyelonephritis, pelvic inflammatory disease, bone joint infection, skin soft-tissue infection, the central nervous system infection etc. of being widely used in.
In the research of medicine, crystal formation research is a very important part.The same medicine, different crystal formations, its character may have very large difference, even has distinct drug effect.Therefore, the research of the crystal formation of medicine also is the focus of present medicament research and development.
Chinese patent CN101289458 discloses refining process for crude product of ceftriaxone sodium, this technique is that crude product of ceftriaxone sodium is dissolved in the water for injection, add the ceftriaxone sodium crystal seed, then add the insoluble organic solvent Virahol of ceftriaxone sodium, obtain the ceftriaxone sodium finished product.
A kind of technique of ceftriaxone sodium crystallization has been described in " ceftriaxone sodium crystallization process research " that the people such as Huifen LI deliver, this technique is that crude product of ceftriaxone sodium is dissolved in the mixed solvent of purified water and acetone, add the ceftriaxone sodium crystal seed behind the activated carbon decolorizing, drip acetone behind the crystallization, finally obtain the ceftriaxone sodium powder of white.
The refining method of a kind of ceftriaxone sodium is disclosed in " improvement of Recrystal Method of Ceftriaxone Sodium " that the people such as Wang Donghai deliver, the method is that ceftriaxone sodium is dissolved in the mixed solvent of the purified water that is added with sodium bisulfite and dehydrated alcohol, then add the ceftriaxone sodium crystal seed, drip dehydrated alcohol behind the crystallization, obtain white crystalline ceftriaxone sodium powder, crystal formation is thick.Give ceftriaxone sodium acetone crystallization control experiment in the article, the dehydrated alcohol that is about in the above-mentioned process for purification all changes acetone into, obtains at last white crystalline ceftriaxone sodium powder, and crystal formation is very thin.
All the crystal formation of ceftriaxone sodium is not studied in the above-mentioned document.
Provided a kind of collection of illustrative plates of ceftriaxone sodium crystal form X-ray powder diffraction in " Non-isothermal Dehydration Kinetics of Ceftriaxone Disodium Hemiheptahydrate " that the people such as Zhang Chuntao deliver, the peak value of its 2 θ angle is respectively: 11.9364,8.0076,7.0981,5.7638,5.1099,4.8355,4.7014,4.4579,4.1992,3.9140,3.7417,3.5366,3.3336,3.1597,3.0254,2.9062,2.6452,2.5116,2.3469,2.2662,2.0906,2.0404,1.9681.
In " research of ceftriaxone sodium crystalline structure and crystal habit predicting " literary composition that the people such as Zhang Chuntao deliver, provided a kind of data of ceftriaxone sodium crystal form X-ray powder diffraction, specific as follows:
Do not provide the corresponding preparation method of ceftriaxone sodium crystal in above two pieces of documents.
This shows, although ceftriaxone sodium is widely used kind in the cephalosporin medicament, its crystal formation research and imperfection remain further to be explored.
Summary of the invention
Technical problem to be solved by this invention provides ceftriaxone sodium crystal and preparation method thereof, and the method need not to add crystal seed, and is easy and simple to handle, and the crystal formation for preparing is needle-like or sheet.
The inventor is through long-term and unremitting experimental study, by regulating the consumption of acetone, crystallization control temperature and crystallization time change the crystal solution degree of supersaturation to reach, affect the purpose of crystallization nucleation and crystal production speed, thereby obtained to be suitable for medicinal ceftriaxone sodium novel crystal form.
Purpose of the present invention is achieved through the following technical solutions.
A kind of ceftriaxone sodium crystal uses Cu-K α radiation, with 2 θ angles (°) the X-diffraction of expression having the peak with upper/lower positions:
(1) 19.0 ± 0.2,24.6 ± 0.2; Perhaps
(2) 4.8 ± 0.2,18.6 ± 0.2,19.0 ± 0.2,24.6 ± 0.2; Perhaps
（3）4.8±0.2、11.5±0.2、15.5±0.2、17.4±0.2、18.6±0.2、19.0±0.2、20.0±0.2、24.6±0.2、25.1±0.2、28.2±0.2、28.9±0.2、35.9±0.2、44.3±0.2、49.5±0.2。
Ceftriaxone sodium crystal of the present invention, means of differential scanning calorimetry heat absorption maximum value is 270-273 ℃.
In the preferred embodiment of the present invention, described ceftriaxone sodium crystal uses Cu-K α radiation, with 2 θ angles (°) the X-diffraction of expression further also having the peak with upper/lower positions:
(1) 10.5 ± 0.2,22.9 ± 0.2,23.3 ± 0.2,27.1 ± 0.2,32.8 ± 0.2; Perhaps
(2) 9.4 ± 0.2,10.5 ± 0.2,22.9 ± 0.2,23.3 ± 0.2,27.1 ± 0.2,29.2 ± 0.2,32.8 ± 0.2; Perhaps
（3）9.4±0.2、10.5±0.2、12.2±0.2、13.0±0.2、14.0±0.2、21.4±0.2、22.9±0.2、23.3±0.2、25.7±0.2、27.1±0.2、29.2±0.2、32.8±0.2、37.6±0.2、39.9±0.2、47.4±0.2。
In preferred another embodiment of the present invention, described ceftriaxone sodium crystal uses Cu-K α radiation, with 2 θ angles (°) the X-diffraction of expression further also having the peak with upper/lower positions:
(1) 11.2 ± 0.2,22.5 ± 0.2,24.0 ± 0.2,26.8 ± 0.2,29.5 ± 0.2,33.8 ± 0.2; Perhaps
(2) 11.2 ± 0.2,12.5 ± 0.2,22.5 ± 0.2,24.0 ± 0.2,26.8 ± 0.2,29.5 ± 0.2,33.8 ± 0.2; Perhaps
（3）7.5±0.2、11.2±0.2、12.5±0.2、15.1±0.2、22.5±0.2、24.0±0.2、26.8±0.2、29.5±0.2、30.9±0.2、33.8±0.2、38.4±0.2、39.3±0.2、40.6±0.2、41.6±0.2、43.2±0.2、49.1±0.2。
The preparation method of ceftriaxone sodium crystal of the present invention operates as follows:
A. get crude product of ceftriaxone sodium, add in the purified water, temperature control stirring to solid all dissolves, and filters filtrate for later use;
B. stir, temperature control drips acetone in the filtrate for preparing to step a, gets mixed solution;
C. the mixed solution cooling that step b is prepared is left standstill, and gets crystal solution;
D. the crystal solution suction filtration that step c is prepared, washing, drying gets the ceftriaxone sodium crystal.
Preparation method of the present invention, crude product of ceftriaxone sodium and dissolving are 1:10-16 with the weight ratio of purified water among the step a, preferred 1:10 prepares the needle-like crystal formation.
Preparation method of the present invention, crude product of ceftriaxone sodium and dissolving are 1:2-5 with the weight ratio of purified water among the step a, preferred 1:3 prepares the sheet crystal formation.
Above-mentioned preparation method, temperature control is to 20-25 ℃ when dissolving among the step a.
Above-mentioned preparation method, among the step b among the consumption of acetone and the step a consumption volume ratio of purified water be 0.5-4:1.
Above-mentioned preparation method, dripping the used time of acetone among the step b is 0.5-2h.
Above-mentioned preparation method is cooled to 20-25 ℃ or 5-10 ℃ among the step c.
Above-mentioned preparation method, time of repose is 8-12h among the step c, preferred 10h.
Ceftriaxone sodium crystal of the present invention, content prove that through long-term and accelerated test it has good stability more than 94%, meet the requirement of pharmacopeia, can be used as bulk drug and use.The preparation method of ceftriaxone sodium crystal of the present invention need not add crystal seed in addition, and is simple to operate, and yield is suitable for suitability for industrialized production and uses more than 84%.
Description of drawings
Fig. 1 is the collection of illustrative plates of ceftriaxone sodium crystal form X-ray powder diffraction of providing among " the Non-isothermal Dehydration Kinetics of Ceftriaxone Disodium Hemiheptahydrate " that the people such as Zhang Chuntao delivers in the background technology.
Fig. 2 is the DSC-DTG-DG collection of illustrative plates of embodiment 1 gained ceftriaxone sodium crystal.
Fig. 3 is the X-diffracting spectrum of embodiment 1 gained ceftriaxone sodium crystal.
Fig. 4 is the DSC-DTG-DG collection of illustrative plates of embodiment 6 gained ceftriaxone sodium crystals.
Fig. 5 is the X-diffracting spectrum of embodiment 6 gained ceftriaxone sodium crystals.
Embodiment
Get crude product of ceftriaxone sodium 10g, be added in the 100mL purified water, temperature control 20-25 ℃, stir the lower acetone 250mL that drips, time spent 1.5h stops after dropwising stirring, 20-25 ℃ leaves standstill 10h, and suction filtration is with acetone 100mL washing, drain, vacuum-drying gets ceftriaxone sodium solid 9.0g, yield 90%, content is 94.3% after testing, and crystal formation is needle-like.
The products obtained therefrom fusing point is 271 ℃, and the DSC-DTG-DG collection of illustrative plates is seen Fig. 2, and X-diffracting spectrum data are as shown in table 1, and the X-diffracting spectrum is seen Fig. 3.
Table 1
| Sequence number | 2θ（°） | Peak intensity (%) |
| 1 | 4.749 | 13.9 |
| 2 | 9.351 | 12.8 |
| 3 | 10.529 | 30.4 |
| 4 | 11.438 | 6.5 |
| 5 | 12.204 | 7.6 |
| 6 | 13.004 | 5.9 |
| 7 | 13.997 | 9.5 |
| 8 | 15.615 | 6.9 |
| 9 | 17.392 | 15.8 |
| 10 | 18.64 | 16.7 |
| 11 | 19.019 | 100 |
| 12 | 20.012 | 7.4 |
| 13 | 21.412 | 6.5 |
| 14 | 22.912 | 23 |
| 15 | 23.337 | 45.1 |
| 16 | 24.576 | 44.7 |
| 17 | 25.06 | 6.3 |
| 18 | 25.741 | 6.5 |
| 19 | 27.071 | 22.1 |
| 20 | 28.067 | 15 |
| 21 | 28.88 | 6.9 |
| 22 | 29.2 | 18 |
| 23 | 32.848 | 24.7 |
| 24 | 35.94 | 7.4 |
| 25 | 37.607 | 9.3 |
| 26 | 39.886 | 6.1 |
| 27 | 44.331 | 8 |
| 28 | 47.404 | 5.9 |
| 29 | 49.573 | 7.4 |
Embodiment 2-5
Operate according to embodiment 1 described method, design parameter is as shown in table 2.
Table 2
| Numbering | Crude product of ceftriaxone sodium (g) | Purified water (mL) | Drip acetone (mL) | Drip the time spent (h) | Time of repose (h) | Dwell temperature (℃) | Yield (%) | Content (%) |
|
| Embodiment | |||||||||
| 2 | 10 | 100 | 260 | 2 | 8 | 20-25 | 85.6 | 94.2 | With |
| Embodiment 3 | 9 | 100 | 270 | 0.5 | 12 | 20-25 | 87.4 | 94.3 | With |
| Embodiment 4 | 8 | 80 | 280 | 1.5 | 10 | 5-10 | 84.6 | 94.2 | With |
| Embodiment 5 | 5 | 80 | 310 | 2 | 12 | 5-10 | 86.3 | 94.0 | With |
Get crude product of ceftriaxone sodium 32g, be added in the 100mL purified water, temperature control 20-25 ℃, stir the lower acetone 100mL that drips, time spent 1h stops after dropwising stirring, 5-10 ℃ leaves standstill 12h, and suction filtration is with acetone 200mL washing, drain, vacuum-drying gets ceftriaxone sodium solid 28.7g, yield 89.6%, content is 94.2% after testing, and crystal formation is sheet.
The products obtained therefrom fusing point is 272 ℃, and the DSC-DTG-DG collection of illustrative plates is seen Fig. 4, and X-diffracting spectrum data are as shown in table 3, and the X-diffracting spectrum is seen Fig. 5.
Table 3
| Sequence number | 2θ（°） | Peak intensity (%) |
| 1 | 4.829 | 20.9 |
| 2 | 7.538 | 7.2 |
| 3 | 11.153 | 56.1 |
| 4 | 11.599 | 7.4 |
| 5 | 12.547 | 11.3 |
| 6 | 15.053 | 6.1 |
| 7 | 15.462 | 22.3 |
| 8 | 17.424 | 6.4 |
| 9 | 18.408 | 33.4 |
| 10 | 19.169 | 33.6 |
| 11 | 19.989 | 100 |
| 12 | 22.512 | 26.6 |
| 13 | 24.007 | 48.6 |
| 14 | 24.75 | 56.4 |
| 15 | 25.255 | 7.6 |
| 16 | 26.779 | 39.6 |
| 17 | 28.23 | 6.1 |
| 18 | 28.896 | 25 |
| 19 | 29.531 | 31.1 |
| 20 | 30.863 | 8.6 |
| 21 | 33.815 | 23.8 |
| 22 | 35.76 | 9.8 |
| 23 | 38.361 | 9.6 |
| 24 | 39.27 | 7 |
| 25 | 40.568 | 5.9 |
| 26 | 41.613 | 6.4 |
| 27 | 43.186 | 7.8 |
| 28 | 44.285 | 14.1 |
| 29 | 49.064 | 8 |
| 30 | 49.475 | 10.5 |
Embodiment 7-13
Operate according to embodiment 6 described methods, design parameter is as shown in table 4.
Table 4
| Numbering | Crude product of ceftriaxone sodium (g) | Purified water (mL) | Drip acetone (mL) | Drip the time spent (h) | Time of repose (h) | Dwell temperature (℃) | Yield (%) | Content (%) | Crystal formation |
| Embodiment 7 | 34 | 100 | 80 | 0.5 | 10 | 5-10 | 86.4 | 94.2 | With |
| |
32 | 100 | 100 | 0.5 | 10 | 5-10 | 86.4 | 94.0 | With |
| Embodiment 9 | 31 | 100 | 110 | 1.5 | 8 | 5-10 | 87.9 | 94.1 | With |
| |
30 | 100 | 120 | 1 | 8 | 5-10 | 89.4 | 94.1 | With |
| Embodiment 11 | 29 | 100 | 130 | 1.5 | 12 | 5-10 | 85.3 | 94.2 | With |
| |
28 | 100 | 140 | 0.5 | 10 | 20-25 | 85.6 | 94.1 | With |
| Embodiment 13 | 27 | 100 | 160 | 2 | 12 | 20-25 | 86.3 | 94.3 | With |
In order to investigate the stability of ceftriaxone sodium crystal of the present invention, the inventor has carried out stability test research to the product that embodiment 1-13 prepares, and contrast with ceftriaxone sodium injection that Roche Holding Ag of the former unit of grinding produces, comprise accelerated test and test of long duration two portions, specific as follows.
(1) accelerated test
Get each embodiment sample, press commercially available back, get simultaneously commercially available Roche Holding Ag product, 40 ℃ ± 2 ℃ of temperature, placed 6 months under the condition of relative humidity 75% ± 5%, detect the 1st, 2,3,6 sampling at the end of month respectively, the result is shown in table 5-1, table 5-2, table 5-3, table 5-4, table 5-5.
Table 5-1
Table 5-2
Table 5-3
Table 5-4
Table 5-5
Can find out from the accelerated test result, ceftriaxone sodium crystal product of the present invention respectively detects index without noticeable change, has good stability, and obviously is better than the product of commercially available Roche Holding Ag.
(2) test of long duration
Get each embodiment sample, press commercially available back, get simultaneously the commercially available prod, 25 ℃ ± 2 ℃ of temperature, placed 12 months under the condition of relative humidity 60% ± 10%, detect the 3rd, 6,9,12 sampling at the end of month respectively, the result is shown in table 6-1, table 6-2, table 6-3, table 6-4, table 6-5.
Table 6-1
Table 6-2
Table 6-3
Table 6-4
Table 6-5
Find out from long-term test results, ceftriaxone sodium crystal product of the present invention respectively detects index without noticeable change, has good stability, and obviously is better than the product of commercially available Roche Holding Ag.
Claims (15)
1. a ceftriaxone sodium crystal is characterized in that, uses Cu-K α radiation, with 2 θ angles (°) the X-diffraction of expression having the peak with upper/lower positions:
(1) 19.0 ± 0.2,24.6 ± 0.2; Perhaps
(2) 4.8 ± 0.2,18.6 ± 0.2,19.0 ± 0.2,24.6 ± 0.2; Perhaps
（3）4.8±0.2、11.5±0.2、15.5±0.2、17.4±0.2、18.6±0.2、19.0±0.2、20.0±0.2、24.6±0.2、25.1±0.2、28.2±0.2、28.9±0.2、35.9±0.2、44.3±0.2、49.5±0.2。
2. ceftriaxone sodium crystal according to claim 1 is characterized in that, means of differential scanning calorimetry heat absorption maximum value is 270-273 ℃.
3. ceftriaxone sodium crystal according to claim 1 is characterized in that, uses Cu-K α radiation, with 2 θ angles (°) the X-diffraction of expression further having the peak with upper/lower positions:
(1) 10.5 ± 0.2,22.9 ± 0.2,23.3 ± 0.2,27.1 ± 0.2,32.8 ± 0.2; Perhaps
(2) 9.4 ± 0.2,10.5 ± 0.2,22.9 ± 0.2,23.3 ± 0.2,27.1 ± 0.2,29.2 ± 0.2,32.8 ± 0.2; Perhaps
（3）9.4±0.2、10.5±0.2、12.2±0.2、13.0±0.2、14.0±0.2、21.4±0.2、22.9±0.2、23.3±0.2、25.7±0.2、27.1±0.2、29.2±0.2、32.8±0.2、37.6±0.2、39.9±0.2、47.4±0.2。
4. ceftriaxone sodium crystal according to claim 1 is characterized in that, uses Cu-K α radiation, with 2 θ angles (°) the X-diffraction of expression further having the peak with upper/lower positions:
(1) 11.2 ± 0.2,22.5 ± 0.2,24.0 ± 0.2,26.8 ± 0.2,29.5 ± 0.2,33.8 ± 0.2; Perhaps
(2) 11.2 ± 0.2,12.5 ± 0.2,22.5 ± 0.2,24.0 ± 0.2,26.8 ± 0.2,29.5 ± 0.2,33.8 ± 0.2; Perhaps
（3）7.5±0.2、11.2±0.2、12.5±0.2、15.1±0.2、22.5±0.2、24.0±0.2、26.8±0.2、29.5±0.2、30.9±0.2、33.8±0.2、38.4±0.2、39.3±0.2、40.6±0.2、41.6±0.2、43.2±0.2、49.1±0.2。
5. the preparation method of a ceftriaxone sodium crystal claimed in claim 1 is characterized in that, operates as follows:
A. get crude product of ceftriaxone sodium, add in the purified water, temperature control stirring to solid all dissolves, and filters filtrate for later use;
B. stir, temperature control drips acetone in the filtrate for preparing to step a, gets mixed solution;
C. the mixed solution cooling that step b is prepared is left standstill, and gets crystal solution;
D. the crystal solution suction filtration that step c is prepared, washing, drying gets the ceftriaxone sodium crystal.
6. described preparation method according to claim 5 is characterized in that, crude product of ceftriaxone sodium and dissolving are 1:10-16 with the weight ratio of purified water among the step a.
7. described preparation method according to claim 6 is characterized in that, crude product of ceftriaxone sodium and dissolving are 1:10 with the weight ratio of purified water among the step a.
8. described preparation method according to claim 5 is characterized in that, crude product of ceftriaxone sodium and dissolving are 1:2-5 with the weight ratio of purified water among the step a.
9. described preparation method according to claim 8 is characterized in that, crude product of ceftriaxone sodium and dissolving are 1:3 with the weight ratio of purified water among the step a.
10. described preparation method according to claim 5 is characterized in that, among the step a during dissolving temperature control to 20-25 ℃.
11. described preparation method is characterized in that according to claim 5, among the step b among the consumption of acetone and the step a consumption volume ratio of purified water be 0.5-4:1.
12. described preparation method according to claim 5, dripping the used time of acetone among the step b is 0.5-2h.
13. described preparation method is cooled to 20-25 ℃ or 5-10 ℃ among the step c according to claim 5.
14. described preparation method according to claim 5, time of repose is 8-12h among the step c.
15. described preparation method according to claim 14, time of repose is 10h among the step c.
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| CN106562971B (en) * | 2016-09-30 | 2019-03-22 | 华北制药河北华民药业有限责任公司 | A kind of preparation method of ceftriaxone sodium powder-needle preparation |
| CN109134503A (en) * | 2017-06-14 | 2019-01-04 | 王明 | A kind of four water ceftriaxone sodium compounds |
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| CN108047253A (en) * | 2018-01-04 | 2018-05-18 | 北京红太阳药业有限公司 | A kind of Ceftriaxone Sodium crystal-form compound |
| CN108440569A (en) * | 2018-03-16 | 2018-08-24 | 深圳华润九新药业有限公司 | The preparation method of Ceftriaxone Sodium sphaerocrystal |
| CN110452255A (en) * | 2019-09-05 | 2019-11-15 | 上海龙翔生物医药开发有限公司 | Crystal form of Ceftriaxone Sodium and preparation method thereof |
| CN111909180A (en) * | 2020-09-09 | 2020-11-10 | 瑞阳制药股份有限公司 | Preparation method of ceftriaxone sodium crystal with good stability and high operability |
| CN113105478A (en) * | 2021-03-23 | 2021-07-13 | 广东金城金素制药有限公司 | Monascus sodium compound and crystal form, preparation method and preparation thereof |
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