CN109839460A - A kind of detection method of the Amoxicillin in relation to substance - Google Patents
A kind of detection method of the Amoxicillin in relation to substance Download PDFInfo
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- CN109839460A CN109839460A CN201910191813.6A CN201910191813A CN109839460A CN 109839460 A CN109839460 A CN 109839460A CN 201910191813 A CN201910191813 A CN 201910191813A CN 109839460 A CN109839460 A CN 109839460A
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- mobile phase
- amoxicillin
- related substance
- detecting method
- substance detecting
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Abstract
The present invention relates to pharmaceutical technology field, it is related to a kind of related substance detecting method in Amoxicillin.Sample uses high-efficiency liquid chromatography method for detecting, using mobile phase A and Mobile phase B gradient elution, and records chromatogram.It is party's forensic science, reliable, the related substance in a variety of Amoxicillins can be accurately detected, detection method is easy to operate, separating degree is high, measuring method specificity is strong, testing result is accurately credible.
Description
Technical field
A kind of detection method the present invention relates to pharmaceutical technology field more particularly to Amoxicillin in relation to substance.
Background technique
Amoxicillin be semi-synthetic penicillins wide spectrum beta-lactam antibiotic drug, have significant sterilizing ability and
Cell wall penetration capacity has powerful antibacterial and sterilization to make most of pathogenic G+ bacterium and G- bacterium (including coccus and bacillus)
With wherein to streptococcuses such as streptococcus pneumonia, hemolytic streptococcus, not producing penicillase staphylococcus, enterococcus faecalis etc. and needing
Oxygen gram-positive cocci, the aerobic leather such as escherichia coli, proteus mirabilis, Salmonella, haemophilus influenzae, NEISSERIA GONORRHOEAE
Do not produce the beta lactamase bacterial strain and helicobacter pylori of blue negative bacterium have good antibacterial activity.It is at present using relatively broad
One of semisynthetic penicillin, dosage form includes capsule, tablet, granule etc..
The main organic impurities in Amoxicillin 12, respectively A, B, C, D, E, F, G, H, I, J, L, M, it is miscellaneous from technique
Matter, intermediate products and catabolite.
Detection method of the Amoxicillin in relation to substance in " Chinese Pharmacopoeia " 2015 editions two are as follows:.With the phosphorus of 0.05mol/L
Phthalate buffer (pH value 5.0)-acetonitrile (99:1) is the phosphate buffer (pH value 5.0)-of mobile phase A, 0.05mol/L
Acetonitrile (80:20) is Mobile phase B, gradient elution, flow velocity 1.0mL/min, Detection wavelength 254nm.Elution program are as follows: first to flow
Dynamic phase A- Mobile phase B (92:8) isocratic elution to Amoxicillin appearance finishes, rear according to the form below gradient elution:
There are partial impurities and the not completely separable phenomenon of solvent peak for above-mentioned detection method, and impurity separating degree is low, can draw
Testing result inaccuracy is played, the phenomenon that distortion.
Summary of the invention
The present invention provides a kind of detection method of the Amoxicillin in relation to substance.
The invention is realized in this way a kind of related substance detecting method in Amoxicillin, the detection method use efficient liquid
Chromatography carries out gradient elution using mobile phase A and Mobile phase B, is detected after elution.
Further, the mobile phase A is acetate buffer, citrate buffer, one in phosphate buffer
Kind or a variety of combinations；Mobile phase B is one of acetonitrile, methanol, isopropanol or a variety of combinations.
Further, the pH of the mobile phase A is 4.0~7.0.
Further, the chromatographic column fixed phase filler of the high performance liquid chromatography is octadecylsilane bonded silica
Glue.
Further, the ratio of the gradient elution sequence of the high performance liquid chromatography and mobile phase A and Mobile phase B is such as
Under:
| Time (minute) | 0 | 10 | 35 | 45 | 60 | 65 | 75 |
| Mobile phase A (%) | 100 | 95 | 80 | 85 | 30 | 95 | 100 |
| Mobile phase B (%) | 0 | 5 | 20 | 15 | 70 | 10 | 0 |
。
Further, sample injection high performance liquid chromatograph when, chromatographic condition be injection flow velocity be 0.2ml/min~
2.0ml/min, column temperature are 20 DEG C~40 DEG C, and Detection wavelength is 220nm~280nm.
A kind of Amoxicillin provided by the invention in relation to substance detection method the advantages of be: detection method of the invention
Measure the related substance in Amoxicillin under liquid-phase condition, science, reliable, the related substance in controllable Amoxicillin, detection method operation
Simplicity, separating degree are high, measuring method specificity is strong, testing result is accurately credible.
Detailed description of the invention
Fig. 1 is Amoxicillin impurity mixed chromatogram；
Fig. 2 is the chromatogram of system suitability.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
A kind of detection method of the Amoxicillin in relation to substance, comprising the following steps:
Step 1: test solution, contrast solution and Amoxicillin system suitability of the Amoxicillin in relation to substance are prepared
Contrast solution, the test solution are as follows: take the content of amoxil capsule accurately weighed, during atual detection, Ah
Amdinocillin capsule could alternatively be for Amoxicillin raw material and raw material intermediate products and preparation, and preparation is including but not limited to piece
Agent, capsule, granular preparation finished product and intermediate products related substance.Add mobile phase A to dissolve and quantify dilution and is made in every 1ml
The solution of the 2.0mg containing Amoxicillin, filtration, takes subsequent filtrate as test solution.
Contrast solution: taking Amoxicillin reference substance appropriate, accurately weighed, adds mobile phase A to dissolve and quantifies dilution and is made often
The solution for containing 20 μ g in 1ml, as contrast solution.
Amoxicillin system suitability contrast solution: take Amoxicillin system suitability reference substance and impurity E reference substance suitable
Amount, adds mobile phase A dissolve and dilutes the reference substance of system suitability containing Amoxicillin 1.5mg in every 1ml is made, and impure E is compareed
The solution of 100 μ g of product, as Amoxicillin system suitability solution.
Step 2: test solution obtained by step 1, contrast solution and Amoxicillin system suitability contrast solution are infused
Enter high performance liquid chromatograph, the chromatographic column fixed phase filler of the high performance liquid chromatography is octadecylsilane bonded silica
Then glue carries out gradient elution using mobile phase A and Mobile phase B, is detected after elution, the mobile phase A is 0.05mol/L
Phosphate buffer.
In the actual operation process, the mobile phase A is acetate buffer, citrate buffer, phosphate-buffered
The combination of one or more of liquid, preferably phosphate buffer；Mobile phase B be one of acetonitrile, methanol, isopropanol or
A variety of combinations, preferably acetonitrile.
The pH of the mobile phase A is 4.0~7.0, preferably 4.5~6.8, most preferably 5.5.
The gradient elution sequence of the high performance liquid chromatography is as follows:
| Time (minute) | 0 | 10 | 35 | 45 | 60 | 65 | 75 |
| Mobile phase A (%) | 100 | 95 | 80 | 85 | 30 | 95 | 100 |
| Mobile phase B (%) | 0 | 5 | 20 | 15 | 70 | 10 | 0 |
Wherein, mobile phase A is 0.05mol/L potassium dihydrogen phosphate, and Mobile phase B is acetonitrile.
When injecting high performance liquid chromatograph, chromatographic condition is that injection flow velocity is 0.8ml/min, and column temperature is 30 DEG C, sample introduction body
Product is 20 μ L, Detection wavelength 254nm.
System suitability:
System suitability: it takes Amoxicillin system suitability reference substance and impurity E reference substance appropriate, mobile phase A is added to dissolve
And the solution that the reference substance of system suitability containing Amoxicillin 1.5mg, 100 μ g of impurity E reference substance in every 1ml is made is diluted, as
Amoxicillin system suitability solution.
Measurement: precision measures above-mentioned each 20 μ l of solution, is injected separately into liquid chromatograph, records chromatogram.Referring to Fig. 2,
Fig. 2 is the chromatogram of system suitability.
Peak sequence is followed successively by impurity D, Amoxicillin, E, C, J, Amoxicillin closed loop tripolymer, and the separating degree at each peak is big
In 1.5.
Detection method of the invention measures the related substance in Amoxicillin, science, reliable, controllable A Moxi under liquid-phase condition
The related substance of woods, detection method is easy to operate, separating degree is high, measuring method specificity is strong, testing result is accurately credible.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of related substance detecting method in Amoxicillin, which is characterized in that the detection method uses high performance liquid chromatograph, adopts
Gradient elution detection is carried out with mobile phase A and Mobile phase B.
2. the related substance detecting method in Amoxicillin according to claim 1, which is characterized in that the mobile phase A is vinegar
The combination of one or more of phthalate buffer, citrate buffer, phosphate buffer；Mobile phase B is acetonitrile, first
One of alcohol, isopropanol or a variety of combinations.
3. the related substance detecting method in Amoxicillin described in -2 any one according to claim 1, which is characterized in that the stream
The pH of dynamic phase A is 4.0~7.0.
4. the related substance detecting method in Amoxicillin according to claim 3, which is characterized in that the high performance liquid chromatography
The chromatographic column fixed phase filler of method is octadecylsilane chemically bonded silica.
5. the related substance detecting method in Amoxicillin according to claim 4, which is characterized in that the high performance liquid chromatography
The gradient elution sequence and mobile phase A of method and the ratio of Mobile phase B are as follows:
。
6. the related substance detecting method in Amoxicillin described in -5 according to claim 1, which is characterized in that sample injects efficient liquid
When chromatography, chromatographic condition is that injection flow velocity is 0.2ml/min~2.0ml/min, and column temperature is 20 DEG C~40 DEG C, Detection wavelength
For 220nm~280nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910191813.6A CN109839460A (en) | 2019-03-14 | 2019-03-14 | A kind of detection method of the Amoxicillin in relation to substance |
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| CN201910191813.6A CN109839460A (en) | 2019-03-14 | 2019-03-14 | A kind of detection method of the Amoxicillin in relation to substance |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461954A (en) * | 2020-11-11 | 2021-03-09 | 广州市力鑫药业有限公司 | Impurity detection method for amoxicillin bulk drug |
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|---|---|---|---|---|
| CN101776675A (en) * | 2008-08-27 | 2010-07-14 | 广州联创思远利生物科技有限公司 | Novel detection method of injection use compound amoxicillin sodium and clavulanate potassium |
| CN107589212A (en) * | 2017-06-01 | 2018-01-16 | 合肥远志医药科技开发有限公司 | A kind of detection method of amoxil capsule about material |
| CN108693293A (en) * | 2018-07-25 | 2018-10-23 | 广州白云山医药集团股份有限公司白云山制药总厂 | The method for detecting impurity in amoxicillin granules |
| WO2018204317A1 (en) * | 2017-05-02 | 2018-11-08 | Lubrizol Advanced Materials, Inc. | Improved extended release highly loaded drug compositions |
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2019
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776675A (en) * | 2008-08-27 | 2010-07-14 | 广州联创思远利生物科技有限公司 | Novel detection method of injection use compound amoxicillin sodium and clavulanate potassium |
| WO2018204317A1 (en) * | 2017-05-02 | 2018-11-08 | Lubrizol Advanced Materials, Inc. | Improved extended release highly loaded drug compositions |
| CN107589212A (en) * | 2017-06-01 | 2018-01-16 | 合肥远志医药科技开发有限公司 | A kind of detection method of amoxil capsule about material |
| CN108693293A (en) * | 2018-07-25 | 2018-10-23 | 广州白云山医药集团股份有限公司白云山制药总厂 | The method for detecting impurity in amoxicillin granules |
Non-Patent Citations (3)
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|---|
| CAI SHAN-YING 等: "Chromatographic determination of high-molecular weight impurities in amoxicillin", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 殷果 等: "国产注射用阿莫西林钠中主要杂质分析", 《药物分析杂志》 * |
| 缪文玲 等: "阿莫西林克拉维酸钾片的杂质谱研究", 《中国药学杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461954A (en) * | 2020-11-11 | 2021-03-09 | 广州市力鑫药业有限公司 | Impurity detection method for amoxicillin bulk drug |
| CN112461954B (en) * | 2020-11-11 | 2021-07-09 | 广州市力鑫药业有限公司 | Impurity detection method for amoxicillin bulk drug |
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