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Crystal form of ceftriaxone sodium and preparation method for crystal form

A technology of ceftriaxone sodium and crystal form, which is applied in the field of medicine, can solve problems such as imperfect crystal form research, and achieve the effect of good stability and simple operation

Inactive Publication Date: 2013-01-16
石药集团中诺药业(石家庄)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] It can be seen from this that although ceftriaxone sodium is a widely used variety in cephalosporin drugs, its crystal form research is not perfect and needs to be further explored

Method used

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  • Crystal form of ceftriaxone sodium and preparation method for crystal form
  • Crystal form of ceftriaxone sodium and preparation method for crystal form
  • Crystal form of ceftriaxone sodium and preparation method for crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Take 10g of crude ceftriaxone sodium, dissolve it into 100mL of purified water, control the temperature at 20-25°C, add 250mL of acetone dropwise under stirring for 1.5h, stop stirring after the addition is complete, let stand at 20-25°C for 10h, and filter with suction , washed with acetone 100mL, drained, and vacuum-dried to obtain 9.0 g of ceftriaxone sodium as a solid, with a yield of 90%, the detected content was 94.3%, and the crystal form was needle-like.

[0052] The resulting product has a melting point of 271°C, and the DSC-DTG-DG spectrum is shown in figure 2 , X-diffraction spectrum data are shown in Table 1, X-diffraction spectrum see image 3 .

[0053] Table 1

[0054] serial 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 ...

Embodiment 2-5

[0056] Operate according to the method described in Example 1, and the specific parameters are shown in Table 2.

[0057] Table 2

[0058] serial number Crude ceftriaxone sodium (g) Purified water (mL) Add acetone dropwise (mL) Dropping time (h) Standing time (h) Standing temperature (°C) Yield (%) content(%) crystal form Example 2 10 100 260 2 8 20-25 85.6 94.2 Same as Example 1 Example 3 9 100 270 0.5 12 20-25 87.4 94.3 Same as Example 1 Example 4 8 80 280 1.5 10 5-10 84.6 94.2 Same as Example 1 Example 5 5 80 310 2 12 5-10 86.3 94.0 Same as Example 1

Embodiment 6

[0060] Take 32g of crude ceftriaxone sodium, dissolve it into 100mL of purified water, control the temperature at 20-25°C, add 100mL of acetone dropwise under stirring for 1h, stop stirring after the addition is complete, let stand at 5-10°C for 12h, and filter with suction. Wash with 200 mL of acetone, pump dry, and dry in vacuo to obtain 28.7 g of ceftriaxone sodium as a solid, with a yield of 89.6%. The detected content is 94.2%, and the crystal form is flake.

[0061] The melting point of the obtained product is 272°C, and the DSC-DTG-DG spectrum is shown in Figure 4 , the X-diffraction pattern data are shown in Table 3, and the X-diffraction pattern is shown in Figure 5 .

[0062] table 3

[0063] serial 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...

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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 [0001] The invention belongs to the technical field of medicine, and relates to a crystal form of medicine and a preparation method thereof, in particular to a crystal form of ceftriaxone sodium and a preparation method thereof. Background technique [0002] Ceftriaxone sodium belongs to the third generation of cephalosporins for injection, researched and developed by Roche, Switzerland, and its chemical name is (6R, 7R)-7-[[(2-amino-4-thiazolyl)(methoxysubstance Amino)acetyl]amino]-8-oxo-3-[[(1,2,5,6-tetrahydro-2methyl-5,6-dioxo-1,2,4-triazine-3 -yl)thio]methyl]-5-thio-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid disodium salt triple hemihydrate, its structural formula is as follows: [0003] . [0004] Ceftriaxone sodium is a semi-synthetic cephalosporin, which exerts antibacterial effect by inhibiting the synthesis of bacterial cell walls, and has strong antibacterial activity against most Gram-positive bacteria and Gram-negative bacteria. It is mai...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
Inventor 杨梁卢华姚兵安志强郝金恒齐雁鸿李建强徐永龙袁军才戚桂军胡艳茹
Owner 石药集团中诺药业(石家庄)有限公司
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