CN103713080A - Method for detecting content of gamithromycin - Google Patents
Method for detecting content of gamithromycin Download PDFInfo
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- CN103713080A CN103713080A CN201310745236.3A CN201310745236A CN103713080A CN 103713080 A CN103713080 A CN 103713080A CN 201310745236 A CN201310745236 A CN 201310745236A CN 103713080 A CN103713080 A CN 103713080A
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- meter mycin
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Abstract
The invention provides a method for detecting the content of gamithromycin. The method comprises the steps: dissolving a gamithromycin sample to be detected by a flowing phase, and performing liquid phase chromatogram quantitative analysis by using a DAD (Dioxide Array Detector) detector adopting C8 and C18 chromatographic columns, wherein chromatographic conditions are as follows: the flowing phase is as follows: a weight ratio of acetonitrile to 0.025mol/ml dipotassium phosphate solution (PH8-8.5) is 70:30, a flow velocity is 1.00-2.00ml/min, and a detection wavelength is 210-230nm. The method is accurate and simple, and is good in reproducibility and high in sensitivity.
Description
Technical field
The present invention relates to a kind of medicament contg detection method, especially a kind of detection method of content that adds meter mycin.
Background technology
Add a meter mycin (Gamithromycin) and belong to macrolide antibiotics, be mainly used in treating the cattle infected disease that the bacterial pathogens such as pasteurella haemolytica, pasteurella multocida and Histophilus cause, have and absorb the advantages such as fast, the interior widely distributed residual quantity of body is low, security is high, and the report that has no adverse reaction temporarily has wide practical use on veterinary clinic.
The synthetic route that adds meter mycin is as follows:
Yet in exploitation, add in the process of meter mycin, this chemicals does not have ready-made determination and analysis method, and this present situation makes this medicine there is no unified standard, has hindered greatly application and the popularization of this medicine.Therefore it is very necessary, setting up a set of effective, stable detection method of content.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of detection method of content that adds meter mycin.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of detection method of content that adds meter mycin, adopt liquid chromatography to analyze, concrete steps are: mobile phase dissolves meter mycin sample that adds to be detected, take C8, C18 as chromatographic column, with DAD detecting device, carry out chromatogram quantitative analysis of the liquid phase, its chromatographic condition is: mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8-8.5)=70:30, flow velocity: 1.00-2.00ml/min, detects wavelength: 210-230nm.
Preferably, the above-mentioned detection method of content that adds meter mycin, described mobile phase dissolves to be detected adding after meter mycin sample, and adding a meter mycin sample concentration is 0.006mg/ml-1.523mg/ml.
Preferably, the above-mentioned detection method of content that adds meter mycin, described chromatographic condition is: mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8.2)=70:30, flow velocity: 1.00ml/min, detects wavelength: 210nm.
Preferably, the above-mentioned detection method of content that adds meter mycin, is added the mould cellulose content of rice and carries out quantitatively adding by external standard method in meter mycin sample.
The invention has the beneficial effects as follows:
The above-mentioned detection method of content that adds meter mycin, by liquid chromatography, carry out analyzing and testing, external standard method is carried out quantitatively adding the mould cellulose content of rice in sample, described method is accurate, simple, favorable reproducibility, highly sensitive, when adding meter mycin between 0.004mg/ml-1.2mg/ml time, all have good linear relationship, its linearly dependent coefficient is 0.9997.
Accompanying drawing explanation
Fig. 1 adds a meter liquid chromatogram for mycin reference substance;
Fig. 2 is the liquid chromatogram that adds meter mycin;
Fig. 3 adds a meter liquid chromatogram for mycin parenteral solution;
Fig. 4 adds a meter liquid chromatogram for mycin soluble powder.
Embodiment
In order to make those skilled in the art better understand technical scheme of the present invention, below in conjunction with embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
I instrument and equipment and starting material:
Agilent 1260 chromatographic analyzer of liquid phase, are equipped with DAD diode array detector, OPENLAB chromatographic work station, C
8, C
18chromatographic column;
Acetonitrile (HPLC level), dipotassium hydrogen phosphate (AG), secondary deionized water, add a meter mycin reference substance (being provided by Nat'l Pharmaceutical & Biological Products Control Institute), add a meter mycin (commercially available).
II adds a meter preparation for mycin analytic sample:
1, take 0.01021g and add meter mycin to 10ml volumetric flask, add 2ml acetonitrile and dissolve, with mobile phase, be diluted to scale, shake up.
2, precision takes and adds in meter mycin reference substance 10.02 ㎎ to 10ml volumetric flasks, adds 2ml acetonitrile and dissolves, and with mobile phase, is diluted to scale, shakes up.
3, chromatographiccondition:
Mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8.2)=70:30;
Flow velocity: 1.00ml/min;
Detect wavelength: 210nm;
Sample size: 20 μ l.
4, by external standard method, calculate and add meter content of mycin sample a: a=A
samplem
mark/ A
markm
sample* 100%=10.02*1363.6/1390.6*10.21*100%=96.2% (the results are shown in Figure 1 and Fig. 2)
Embodiment 2
I instrument and equipment and starting material:
Agilent 1260 chromatographic analyzer of liquid phase, are equipped with DAD diode array detector, OPENLAB chromatographic work station, C
8, C
18chromatographic column;
Acetonitrile (HPLC level), dipotassium hydrogen phosphate (AG), secondary deionized water, add a meter mycin reference substance (being provided by Nat'l Pharmaceutical & Biological Products Control Institute), add a meter mycin parenteral solution (commercially available, specification 15g:100ml).
II adds a meter preparation for mycin analytic sample:
1, pipette 1ml and add meter mycin parenteral solution to 10ml volumetric flask, with mobile phase, be diluted to scale, shake up; With appropriate mobile phase dilute solution to 1 ㎎/ml progressively, with filtering with microporous membrane gained solution.
2, precision takes and adds in meter mycin reference substance 10.15 ㎎ to 10ml volumetric flasks, adds 1-2ml acetonitrile and dissolves, and with mobile phase, is diluted to scale, shakes up, with filtering with microporous membrane gained solution.
3, chromatographiccondition:
Mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8.2)=70:30;
Flow velocity: 1.00ml/min;
Detect wavelength: 210nm;
Sample size: 20 μ l.
4, by external standard method, calculate and add a meter content for mycin parenteral solution.A=A
samplem
mark/ 1500A
mark* 100%=1370.3*10.15/10*1390.6*100%=100.02%(the results are shown in Figure 1 and Fig. 3)
Embodiment 3
I instrument and equipment and starting material:
Agilent 1260 chromatographic analyzer of liquid phase, are equipped with DAD diode array detector, OPENLAB chromatographic work station, C
8, C
18chromatographic column;
Acetonitrile (HPLC level), dipotassium hydrogen phosphate (AG), secondary deionized water, add a meter mycin reference substance (being provided by Nat'l Pharmaceutical & Biological Products Control Institute), add a meter mycin pre-mixing agent (commercially available, specification 15g:100g).
II adds a meter preparation for mycin analytic sample:
1, pipette 1.04g and add meter mycin pre-mixing agent to 10ml volumetric flask, with mobile phase, be diluted to scale, shake up, with appropriate mobile phase dilute solution to 1 ㎎/ml progressively, with filtering with microporous membrane gained solution.
2, precision takes and adds in meter mycin reference substance 10.11 ㎎ to 10ml volumetric flasks, adds 1-2ml acetonitrile and dissolves, and with mobile phase, is diluted to scale, shakes up, with filtering with microporous membrane gained solution.
3, chromatographiccondition:
Mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8.2)=70:30;
Flow velocity: 1.00ml/min;
Detect wavelength: 210nm;
Sample size: 20 μ l.
4, by external standard method, calculate and add a meter content for mycin parenteral solution.A=A
samplem
mark/ 10.4A
mark* 100%=1349.2*10.11/10.4*1390.6*100%=94.3%(the results are shown in Figure 1 and Fig. 4)
Above-mentioned detailed description of this kind of detection method of content that adds meter mycin being carried out with reference to embodiment; illustrative rather than determinate; can list several embodiment according to institute's limited range; therefore in the variation and the modification that do not depart under general plotting of the present invention, within should belonging to protection scope of the present invention.
Claims (4)
1. a detection method of content that adds meter mycin, it is characterized in that: adopt liquid chromatography to analyze, concrete steps are: mobile phase dissolves meter mycin sample that adds to be detected, take C8, C18 as chromatographic column, with DAD detecting device, carry out chromatogram quantitative analysis of the liquid phase, its chromatographic condition is: mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8-8.5)=70:30, flow velocity: 1.00-2.00ml/min, detects wavelength: 210-230nm.
2. the detection method of content that adds meter mycin according to claim 1, is characterized in that: described mobile phase dissolves to be detected adding after meter mycin sample, and adding a meter mycin sample concentration is 0.006mg/ml-1.523mg/ml.
3. the detection method of content that adds meter mycin according to claim 1, it is characterized in that: described chromatographic condition is: mobile phase: acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (PH8.2)=70:30, flow velocity: 1.00ml/min, detects wavelength: 210nm.
4. the detection method of content that adds meter mycin according to claim 1, is characterized in that: by external standard method, to adding, added the mould cellulose content of rice carry out quantitatively in meter mycin sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310745236.3A CN103713080A (en) | 2013-12-25 | 2013-12-25 | Method for detecting content of gamithromycin |
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|---|---|---|---|
| CN201310745236.3A CN103713080A (en) | 2013-12-25 | 2013-12-25 | Method for detecting content of gamithromycin |
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| CN103713080A true CN103713080A (en) | 2014-04-09 |
Family
ID=50406223
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535693A (en) * | 2015-01-21 | 2015-04-22 | 天津市中升挑战生物科技有限公司 | Content detection method of gamithromycin |
| CN107525875A (en) * | 2017-09-15 | 2017-12-29 | 华北制药集团动物保健品有限责任公司 | A kind of detection method of Gamithromycin about material |
| CN107632102A (en) * | 2017-09-13 | 2018-01-26 | 华北制药集团动物保健品有限责任公司 | A kind of detection method of Gamithromycin content |
| CN107764906A (en) * | 2016-08-22 | 2018-03-06 | 洛阳惠中兽药有限公司 | A kind of detection method of content of Gamithromycin |
| CN108567790A (en) * | 2017-03-10 | 2018-09-25 | 洛阳惠中兽药有限公司 | A kind of Gamithromycin pharmaceutical composition and its application |
| CN111778215A (en) * | 2020-07-08 | 2020-10-16 | 江南大学 | Hybridoma cell strain secreting gamithromycin monoclonal antibody and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1262686A (en) * | 1997-07-08 | 2000-08-09 | 生物化学股份有限公司 | Organic compound |
| CN1411465A (en) * | 1999-12-20 | 2003-04-16 | 梅瑞尔公司 | Method for preparing and isolating 9-deoxo-9 (Z)-hydroxyiminoerythromycin A |
| CN102239174A (en) * | 2008-10-24 | 2011-11-09 | 梅里亚有限公司 | Method of synthesizing macrolide compounds |
-
2013
- 2013-12-25 CN CN201310745236.3A patent/CN103713080A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1262686A (en) * | 1997-07-08 | 2000-08-09 | 生物化学股份有限公司 | Organic compound |
| CN1411465A (en) * | 1999-12-20 | 2003-04-16 | 梅瑞尔公司 | Method for preparing and isolating 9-deoxo-9 (Z)-hydroxyiminoerythromycin A |
| CN102239174A (en) * | 2008-10-24 | 2011-11-09 | 梅里亚有限公司 | Method of synthesizing macrolide compounds |
Non-Patent Citations (4)
| Title |
|---|
| R. A. HUANG ET AL.: "Pharmacokinetics of gamithromycin in cattle with comparison of plasma and lung tissue concentrations and plasma antibacterial activity", 《J. VET. PHARMACOL. THERAP.》 * |
| 容永欢: "高效液相色谱法测定阿奇霉素在其分散片中的含量", 《中南药学》 * |
| 王建华 等: "一步法合成9-去氧-8a-氮杂-8a-同型红霉素A", 《合成化学》 * |
| 薛红: "大环内酯类抗生素质量研究的几个重点", 《北方药学》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535693A (en) * | 2015-01-21 | 2015-04-22 | 天津市中升挑战生物科技有限公司 | Content detection method of gamithromycin |
| CN107764906A (en) * | 2016-08-22 | 2018-03-06 | 洛阳惠中兽药有限公司 | A kind of detection method of content of Gamithromycin |
| CN108567790A (en) * | 2017-03-10 | 2018-09-25 | 洛阳惠中兽药有限公司 | A kind of Gamithromycin pharmaceutical composition and its application |
| CN107632102A (en) * | 2017-09-13 | 2018-01-26 | 华北制药集团动物保健品有限责任公司 | A kind of detection method of Gamithromycin content |
| CN107525875A (en) * | 2017-09-15 | 2017-12-29 | 华北制药集团动物保健品有限责任公司 | A kind of detection method of Gamithromycin about material |
| CN111778215A (en) * | 2020-07-08 | 2020-10-16 | 江南大学 | Hybridoma cell strain secreting gamithromycin monoclonal antibody and application thereof |
| CN111778215B (en) * | 2020-07-08 | 2021-11-12 | 江南大学 | Hybridoma cell strain secreting gamithromycin monoclonal antibody and application thereof |
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Application publication date: 20140409 |