CN105116076B - A kind of detection method of Cefodizime Sodium about material - Google Patents
A kind of detection method of Cefodizime Sodium about material Download PDFInfo
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- CN105116076B CN105116076B CN201510624851.8A CN201510624851A CN105116076B CN 105116076 B CN105116076 B CN 105116076B CN 201510624851 A CN201510624851 A CN 201510624851A CN 105116076 B CN105116076 B CN 105116076B
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- cefodizime
- mobile phase
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- cefodizime sodium
- sodium
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Abstract
The present invention relates to a kind of Cefodizime Sodium about the detection method of material, diammonium hydrogen phosphate and acetonitrile is used to carry out gradient elution for mobile phase, achievable Cefodizime is efficiently separated with relevant material.
Description
Technical field
The present invention relates to a kind of Cefodizime Sodium about material detection method.
Background technology
Cefodizime Sodium (cefodizime) as the 3rd generation cynnematin, in the world first by German Hoechst
Roussel Developeies, went through in Japan's listing (trade name in 1990:Neucef), go through within 1994
In importer, the existing nearly 20 years history of domestic and international clinical practice.
The impurity that this product is currently known is：2- sulfydryl -4- methyl-5-thiazole acetic acid（Relevant material I）With the cephalo of Δ -2 ground
Piperazine（Relevant material II）.
The existing liquid phase testing conditions of Cefodizime Sodium are with phosphate buffer（Take the 87g of potassium dihydrogen phosphate 0. with it is anhydrous
The 22g of disodium hydrogen phosphate 0., is dissolved in water and is diluted to 1000ml, shakes up）With acetonitrile with 920：80 are mixed into mobile phase, isocratic
Wash-out.Though the method can realize efficiently separating for Cefodizime and relevant material, it is difficult to reply acid, alkali, high temperature etc. and adds
The separation of complicated ingredient under fast experimental condition.
The content of the invention
The present invention relates to a kind of new method detected to the relevant material of Cefodizime Sodium：
Need testing solution：Take cefodizime sodium for injection appropriate, dissolved with water for injection and be quantitatively diluted to 0.5mg/ml
Solution；
Mobile phase A：5mmol/L ammonium dibasic phosphate solutions；
Mobile phase B：Acetonitrile；
Chromatographic column：200mm × 4.6 mm, 5 μm；
Filler：C18 alkyl silane bonded silica gels；
Column temperature：25℃；
Detection wavelength：262nm；
Flow velocity：1.0mL/min；
Condition of gradient elution：
| Time/min | Mobile phase A（%） | Mobile phase B（%） |
| 0 | 95 | 5 |
| 15 | 80 | 20 |
| 20 | 80 | 20 |
| 25 | 95 | 5 |
| 30 | 95 | 5 |
The μ l of above-mentioned need testing solution 20 are taken, high performance liquid chromatograph is injected, chromatogram is recorded.
Cefodizime Sodium and relevant material I, relevant material II and trans can be realized using detection method of the invention
Cefodizime is efficiently separated, and separating degree is good, and with good reappearance.
Brief description of the drawings
Fig. 1 is detect the liquid chromatogram for obtaining to Cefodizime Sodium using detection method of the invention.
Specific embodiment
Need testing solution：Take cefodizime sodium for injection appropriate, dissolved with water for injection and be quantitatively diluted to 0.5mg/ml
Solution；
Mobile phase A：5mmol/L ammonium dibasic phosphate solutions；
Mobile phase B：Acetonitrile；
Chromatographic column：200mm × 4.6 mm, 5 μm；
Filler：C18 alkyl silane bonded silica gels；
Column temperature：25℃；
Detection wavelength：262nm；
Flow velocity：1.0mL/min；
Condition of gradient elution：
| Time/min | Mobile phase A（%） | Mobile phase B（%） |
| 0 | 95 | 5 |
| 15 | 80 | 20 |
| 20 | 80 | 20 |
| 25 | 95 | 5 |
| 30 | 95 | 5 |
The μ l of above-mentioned need testing solution 20 are taken, high performance liquid chromatograph is injected, chromatogram is recorded.
The ownership of impurity peaks is differentiated by internal standard method, it is as a result as follows：
| Synergy | RT | Content（%） |
| 2- sulfydryl -4- methyl-5-thiazole acetic acid | 3.280 | 0.11 |
| The Cefodizime of Δ -2 | 6.477 | 0.03 |
| Cefodizime | 7.267 | 99.6 |
| Trans Cefodizime | 10.460 | 0.06 |
Claims (1)
1. detection method of a kind of Cefodizime Sodium about material, it is characterised in that：
Need testing solution：Take cefodizime sodium for injection powder appropriate, dissolved with water for injection and be quantitatively diluted to 0.5mg/ml
Solution；
Mobile phase A：5mmol/L ammonium dibasic phosphate solutions；
Mobile phase B：Acetonitrile；
Chromatographic column：200mm × 4.6 mm, 5 μm；
Filler：C18 alkyl silane bonded silica gels；
Column temperature：25℃；
Detection wavelength：262nm；
Flow velocity：1.0mL/min；
Condition of gradient elution：
The μ l of above-mentioned need testing solution 20 are taken, high performance liquid chromatograph is injected, chromatogram is recorded, impurity peaks are returned by internal standard method
Category is differentiated, as a result as follows：
。
Priority Applications (1)
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|---|---|---|---|
| CN201510624851.8A CN105116076B (en) | 2015-09-28 | 2015-09-28 | A kind of detection method of Cefodizime Sodium about material |
Applications Claiming Priority (1)
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|---|---|---|---|
| CN201510624851.8A CN105116076B (en) | 2015-09-28 | 2015-09-28 | A kind of detection method of Cefodizime Sodium about material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105116076A CN105116076A (en) | 2015-12-02 |
| CN105116076B true CN105116076B (en) | 2017-06-30 |
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|---|---|---|---|
| CN201510624851.8A Active CN105116076B (en) | 2015-09-28 | 2015-09-28 | A kind of detection method of Cefodizime Sodium about material |
Country Status (1)
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109900812A (en) * | 2017-12-07 | 2019-06-18 | 北京济美堂医药研究有限公司 | Cefixime and its detection method in relation to substance |
| CN112067709A (en) * | 2020-07-03 | 2020-12-11 | 海口市制药厂有限公司 | Method for determining cefodizime sodium related substance for injection and application |
| CN113406259A (en) * | 2021-05-28 | 2021-09-17 | 海南海灵化学制药有限公司 | Method for detecting latamoxef sodium impurities |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014107536A1 (en) * | 2013-01-04 | 2014-07-10 | Rempex Pharmaceuticals, Inc. | Boronic acid derivatives and therapeutic uses thereof |
| CN104165949A (en) * | 2014-08-29 | 2014-11-26 | 四川制药制剂有限公司 | Inspection method for cefodizime sodium polymer for injection |
| CN104215714A (en) * | 2014-09-21 | 2014-12-17 | 四川制药制剂有限公司 | Determination method of related substance of cefodizime sodium for injection |
-
2015
- 2015-09-28 CN CN201510624851.8A patent/CN105116076B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014107536A1 (en) * | 2013-01-04 | 2014-07-10 | Rempex Pharmaceuticals, Inc. | Boronic acid derivatives and therapeutic uses thereof |
| CN104165949A (en) * | 2014-08-29 | 2014-11-26 | 四川制药制剂有限公司 | Inspection method for cefodizime sodium polymer for injection |
| CN104215714A (en) * | 2014-09-21 | 2014-12-17 | 四川制药制剂有限公司 | Determination method of related substance of cefodizime sodium for injection |
Non-Patent Citations (5)
| Title |
|---|
| Acidic degradation of cefodizime(THR-221) and structural elucidation of the products.I;Teruyoshi Marunaka 等;《Chem.Pharm.Bull.》;19890228;第37卷(第2期);第367-372页 * |
| HPLC-DAD法对注射用头孢地嗪钠杂质谱的一致性分析研究;刘雁鸣 等;《中国药品标准》;20130630;第14卷(第3期);第170-173页 * |
| HPLC梯度洗脱法测定注射用头孢地嗪钠的有关物质;钟莹 等;《中国抗生素杂志》;20140131;第39卷(第1期);第40-44页 * |
| 头孢地嗪钠含量和有关物测定方法研究;姜晓峰 等;《食品与药品》;20150531;第17卷(第3期);第179-183页 * |
| 注射用头孢地嗪钠中特定杂质巯噻唑酸的含量测定;黄秀芬 等;《今日药学》;20130331;第23卷(第3期);第157-159+162页 * |
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|---|---|
| CN105116076A (en) | 2015-12-02 |
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