CN111443139A - Method for simultaneously detecting relative retention time and peak purity of doxycycline and related substances in doxycycline hydrochloride - Google Patents
Method for simultaneously detecting relative retention time and peak purity of doxycycline and related substances in doxycycline hydrochloride Download PDFInfo
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Abstract
The invention discloses a method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hyclate, belonging to the technical field of detection of finished pharmaceutical products, wherein the method adopts a mode of combining HP L C and DAD to simultaneously detect the relative retention time and the peak purity of doxycycline and related substances in doxycycline hyclate, HP L C adopts a UV detector, the UV detector and the DAD detector are arranged in series, a sample is firstly qualitatively detected by the UV detector and then is subjected to peak purity detection by the DAD detector, and the related substances comprise β -doxycycline, methacycline and oxytetracycline.
Description
Technical Field
The invention belongs to the technical field of medicine finished product detection, and particularly relates to a method for simultaneously detecting the relative retention time and peak purity of doxycycline hydrochloride and related substances in doxycycline hydrochloride.
Background
At present, the prices of the standard products of doxycycline sold in the market and the standard products of related substances, such as the standard products of terramycin, the standard products of metacycline, β -doxycycline are very high, the content and the content of the related substances in the standard products of doxycycline hydrochloride in the Chinese pharmacopoeia 2015 edition are still detected by a UV detector, and the peak purity value of each reference product and the doxycycline peak purity value in doxycycline hydrochloride can not be detected.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride, and the peak purity values of doxycycline, β -doxycycline, methacycline and oxytetracycline can be detected while the relative retention time of doxycycline and related substances in doxycycline hydrochloride is detected.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for simultaneously detecting relative retention time and peak purity of doxycycline and related substances in doxycycline hyclate adopts a mode of combining high performance liquid chromatography (HP L C) and a Diode Array Detector (DAD) to simultaneously detect the relative retention time and peak purity value of doxycycline and related substances in doxycycline hyclate, wherein HP L C adopts an ultraviolet detector (UV), the UV detector and the DAD detector are arranged in series, a sample is firstly qualitatively detected by the UV detector, and then is detected by the DAD detector, and the related substances comprise β -doxycycline, metacycline and oxytetracycline, and the method specifically comprises the following steps:
(1) cleaning a sample injection needle before sample injection, and setting HP L C-DAD detection conditions;
(2) preparing a blank solution, a doxycycline reference substance solution, an β -doxycycline standard solution, a metacycline standard solution, a terramycin reference solution and a mixed solution, wherein the blank solution is a 0.01mo L/L hydrochloric acid solution;
(3) and (3) after 1 needle of the solution in the step (2) is respectively put in, continuously collecting 5 needles of doxycycline control solution, and finishing the detection process.
The method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride comprises the steps of adopting an Xbridge C185 mu m chromatographic column, adopting a specification of 4.6 × mm, adopting a flow rate of 1.0m L/min, adopting a column temperature of 35 ℃, adopting a UV detection wavelength of 280nm, adopting a DAD detection wavelength of 280nm, and adopting a sample injection amount of 20 mu L.
The method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride comprises the steps that a mobile phase of HP L C comprises a solution A and a solution B, the solution A is a mixed solution of triethylamine, a 0.25 mol/L ammonium acetate solution and a 0.1 mol/L disodium ethylene diamine tetraacetate solution, the solution B is acetonitrile, the volume ratio of the solution A to the solution B is 88: 15, the solution A is shaken uniformly during preparation, the pH value is adjusted to 8.8 by glacial acetic acid or ammonia water, then the solution A is mixed with the solution B and degassed for later use, and the volume ratio of the ammonium acetate solution, the disodium ethylene diamine tetraacetate solution and the triethylamine in the solution A is 100: 10: 1.
The method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride comprises the following steps:
(1) weighing doxycycline reference substance 20.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 200.0 μ g/m L;
(2) β -doxycycline standard solution is prepared by weighing β -doxycycline standard 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 100.0 μ g/m L;
(3) weighing a metacycline standard substance 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing to a scale to prepare a L solution with the concentration of 100.0 mu g/m;
(4) weighing oxytetracycline reference substance 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing volume to scale to prepare 100.0 μ g/m L solution;
(5) weighing 20.00mg of doxycycline reference substance, 10.00mg of β -doxycycline reference substance, 10.00mg of metycycline reference substance and 10.00mg of oxytetracycline reference substance, adding 0.01 mol/L hydrochloric acid solution for dissolving and diluting to prepare mixed solution containing 0.1mg of oxytetracycline, methacycline, β -doxycycline and 0.2mg of doxycycline in every 1m L.
The method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride specifically comprises the following steps of:
(1) cleaning a sample injection needle before sample injection, and setting HP L C-DAD detection conditions, wherein the HP L C-DAD detection conditions comprise that a chromatographic column adopts Xbridge C18, the specification is 4.6 × 150mm, 5 mu m, the flow rate is 1.0m L/min, the column temperature is 35 ℃, the UV detection wavelength is 280nm, the DAD detection wavelength is 280nm, the sample injection amount is 20 mu L, the mobile phase of HP L C comprises a solution A and a solution B, the solution A is a mixed solution of triethylamine, 0.25 mol/L ammonium acetate solution and 0.1 mol/L disodium ethylene diamine tetraacetate solution, the solution B is acetonitrile, and the volume ratio of the solution A to the solution B is 88: 15, the solution A is shaken uniformly during preparation, the pH value is adjusted to 8.8 by glacial acetic acid or ammonia water, and then the solution A is mixed with the solution B for standby after degassing;
(2) preparing a blank solution, a doxycycline control solution, an β -doxycycline standard solution, a metacycline standard solution, a terramycin control solution and a mixed solution, wherein the blank solution is a 0.01mo L/L hydrochloric acid solution;
weighing doxycycline reference substance 20.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 200.0 μ g/m L;
β -doxycycline standard solution is prepared by weighing β -doxycycline standard 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 100.0 μ g/m L;
weighing a metacycline standard substance 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing to a scale to prepare a solution with the concentration of 100.0 mu g/m L;
weighing oxytetracycline reference substance 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing to volume to scale to prepare solution with concentration of 100.0 μ g/m L;
weighing 20.00mg of doxycycline reference substance, 10.00mg of β -doxycycline reference substance, 10.00mg of metycycline reference substance and 10.00mg of oxytetracycline reference substance, adding 0.01 mol/L hydrochloric acid solution for dissolving and diluting to prepare mixed solution containing 0.1mg of oxytetracycline, methacycline, β -doxycycline and 0.2mg of doxycycline in every 1m L;
(3) and (3) after 1 needle of the solution in the step (2) is respectively put in, continuously collecting 5 needles of doxycycline control solution, and finishing the detection process.
Has the advantages that: compared with the prior art, the invention has the advantages that:
the method simultaneously detects the relative retention time and the peak purity of the doxycycline and related substances in the doxycycline hydrochloride, solves the problem that the existing detection method cannot reflect the peak purity, can accurately detect the relative retention time of the doxycycline and other related substances in the doxycycline hydrochloride, and can analyze the peak purity of a control solution to ensure the effectiveness of the control solution.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example l
A method for detecting relative retention time and peak purity of doxycycline and related substances in doxycycline hyclate simultaneously adopts a mode of combining HP L C and DAD to detect the relative retention time and peak purity of doxycycline and related substances in doxycycline hyclate simultaneously, wherein HP L C adopts a UV detector, the UV detector and the DAD detector are arranged in series, a sample is firstly qualitatively detected by the UV detector, and then the peak purity is detected by the DAD detector, and the related substances are β -doxycycline, metacycline and oxytetracycline, and the method specifically comprises the following steps:
1. HP L C-DAD detection conditions:
a chromatographic column: XBridge C18;
specification of 4.6 × 150mm, 5 μm;
the flow rate is 1.0ml/min, the column temperature is 35 ℃, the UV detection wavelength is 280nm, the DAD detection wavelength is 280nm, and the sample injection amount is 20 mu L;
and a sample injection needle cleaning mode: cleaning before sample introduction, and defatting other conditions;
the mobile phase is prepared by (0.25 mol/L ammonium acetate solution-0.1 mol/L disodium ethylene diamine tetraacetate solution-triethylamine (100: 10: 1), shaking up, adjusting pH value to 8.8 with glacial acetic acid or ammonia water) -acetonitrile (88: 15 by volume ratio), filtering and degassing.
2. Preparing a blank solution, a doxycycline control solution, an β -doxycycline standard solution, a metacycline standard solution, a terramycin control solution and a mixed solution, wherein the blank solution is a 0.01mo L/L hydrochloric acid solution, and the preparation of the solutions is as follows:
(1) weighing doxycycline reference substance 20.02mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and metering to scale to obtain a solution with concentration of 200.2 μ g/ml and identification of 1#And (3) solution.
(2) β -doxycycline standard solution is prepared by weighing β -doxycycline standard 10.16mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and metering to scale to obtain a solution with concentration of 101.6 μ g/ml and identification of 2 μ g/ml#And (3) solution.
(3) Metacycline standard solution is prepared by weighing 10.05mg to 100.0m L volumetric flask of a Metacycline standard, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and metering to scale to obtain a solution with concentration of 100.5 μ g/ml and identification of 3#And (3) solution.
(4) Oxytetracycline control solution: weighing oxytetracycline reference substance 10.21mg to 100.0mL volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing to volume to obtain a solution with concentration of 102.1 μ g/ml and mark of 4#And (3) solution.
(5) Weighing doxycycline reference substance 20.13mg, β -doxycycline reference substance 10.09mg, mettacycline reference substance 10.17mg and oxytetracycline reference substance 10.06mg, adding 0.01 mol/L hydrochloric acid solution to dissolve and dilute into a mixed solution containing oxytetracycline, metacycline, β -doxycycline 0.1mg and doxycycline 0.2mg in each 1ml, wherein the mark is 5#And (3) solution.
3. Measurement of
Under the condition of 1.0 measurement, the blank solution, 1#、2#、3#、4#、5#After 1 needle of each of the six solutions, control 1 was added#The solution was collected for 5 consecutive needles and the relative retention time of each peak and the peak purity are shown in table 1.
TABLE 1 results for relative retention time of each peak and peak purity
| Name (R) | Retention time (min) | Relative retention time | Peak purity (not less than 980) |
| Oxytetracycline | 3.550 | 0.33 | 999 |
| Metacycline | 6.002 | 0.56 | 1000 |
| β -doxycycline | 7.405 | 0.69 | 1000 |
| Doxycycline | 10.742 | 1 | 1000 |
4. Conclusion
As can be seen from Table 1, the device can detect the relative retention time of doxycycline and related substances in doxycycline hydrochloride, can detect the peak purity values of doxycycline, β -doxycycline, methacycline and oxytetracycline, and can meet the design requirements.
Claims (6)
1. A method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride is characterized in that an HP L C and DAD combined mode is adopted to simultaneously detect the relative retention time and the peak purity value of doxycycline and related substances in doxycycline hydrochloride, wherein an HP L C adopts a UV detector, the UV detector and the DAD detector are arranged in series, a sample is firstly qualitatively detected by the UV detector, and then the peak purity is detected by the DAD detector, and the related substances comprise β -doxycycline, metacycline and oxytetracycline.
2. The method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride according to claim 1, wherein the HP L C specifically comprises the following steps:
(1) cleaning a sample injection needle before sample injection, and setting HP L C-DAD detection conditions;
(2) preparing a blank solution, a doxycycline reference substance solution, an β -doxycycline standard solution, a metacycline standard solution, a terramycin reference solution and a mixed solution, wherein the blank solution is a 0.01mo L/L hydrochloric acid solution;
(3) and (3) after the solutions in the step (2) are respectively injected into 1 needle, continuously collecting the doxycycline control solution for 5 needles, and finishing the detection process.
3. The method for simultaneously detecting the relative retention time and the peak purity of doxycycline hydrochloride and related substances in doxycycline hyclate according to claim 1 or 2, wherein the HP L C-DAD is detected under the conditions that an Xbridge C185 μm chromatographic column is adopted, the specification is 4.6 × 150m, the flow rate is 1.0m L/min, the column temperature is 35 ℃, the UV detection wavelength is 280nm, the DAD detection wavelength is 280nm, and the sample injection amount is 20 μ L.
4. The method for simultaneously detecting the relative retention time and the peak purity of doxycycline hydrochloride and related substances in doxycycline hydrochloride according to claim 1 or 2, wherein the HP L C mobile phase comprises a solution A and a solution B, the solution A is a mixed solution of triethylamine, a 0.25 mol/L ammonium acetate solution and a 0.1 mol/L disodium ethylene diamine tetraacetate solution, the solution B is acetonitrile, the volume ratio of the solution A to the solution B is 88: 15, the solution A is shaken up during preparation, the pH value is adjusted to 8.8 by glacial acetic acid or ammonia water, and then the solution A is mixed with the solution B and is degassed for standby, and the volume ratio of the ammonium acetate solution, the disodium ethylene diamine tetraacetate solution and the triethylamine in the solution A is 100: 10: 1.
5. The method for simultaneously detecting the relative retention time and the peak purity of doxycycline hydrochloride and related substances according to claim 1 or 2, wherein the standard solution is prepared by:
(1) weighing doxycycline reference substance 20.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 200.0 μ g/m L;
(2) β -doxycycline standard solution is prepared by weighing β -doxycycline standard 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 100.0 μ g/m L;
(3) weighing a metacycline standard substance 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing to a scale to prepare a solution with the concentration of 100.0 mu g/m L;
(4) weighing oxytetracycline reference substance 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting, and fixing to volume to scale to prepare solution with concentration of 100.0 μ g/m L;
(5) weighing 20.00mg of doxycycline reference substance, 10.00mg of β -doxycycline reference substance, 10.00mg of metycycline reference substance and 10.00mg of oxytetracycline reference substance, adding 0.01 mol/L hydrochloric acid solution for dissolving and diluting to prepare mixed solution containing 0.1mg of oxytetracycline, methacycline, β -doxycycline and 0.2mg of doxycycline in every 1m L.
6. The method for simultaneously detecting the relative retention time and the peak purity of doxycycline and related substances in doxycycline hydrochloride according to claim 1, wherein the HP L C specifically comprises the following steps:
(1) cleaning a sample injection needle before sample injection, and setting HP L C-DAD detection conditions, wherein the HP L C-DAD detection conditions comprise that a chromatographic column adopts Xbridge C18, the specification is 4.6 × 150mm, the diameter is 5 mu m, the flow rate is 1.0m L/min, the column temperature is 35 ℃, the UV detection wavelength is 280nm, the DAD detection wavelength is 280nm, the sample injection amount is 20 mu L, the mobile phase of HP L C comprises a solution A and a solution B, the solution A is a mixed solution of triethylamine, 0.25 mol/L ammonium acetate solution and 0.1 mol/L disodium ethylene diamine tetraacetate solution, the solution B is acetonitrile, and the volume ratio of the solution A to the solution B is 88: 15, the solution A is shaken uniformly during preparation, the pH value is adjusted to 8.8 by glacial acetic acid or ammonia water, and then the solution A is mixed with the solution B and is degassed for standby;
(2) preparing a blank solution, a doxycycline control solution, an β -doxycycline standard solution, a metacycline standard solution, a terramycin control solution and a mixed solution, wherein the blank solution is a 0.01mo L/L hydrochloric acid solution;
weighing 20.00mg to 100.0m L volumetric flask of doxycycline reference substance, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 200.0 μ g/m L;
β -doxycycline standard solution is prepared by weighing β -doxycycline standard 10.00mg to 100.0m L volumetric flask, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing to volume to scale, and preparing into solution with concentration of 100.0 μ g/m L;
weighing a 10.00 mg-100.0 m L volumetric flask of a Meitacycline standard substance, dissolving the Meitacycline standard substance by using a 0.01 mol/L hydrochloric acid solution, diluting and fixing the volume to a scale to prepare a solution with the concentration of 100.0 mu g/m L;
weighing oxytetracycline reference substance 10.00mg to 100.0m L volumetric flasks, dissolving with 0.01 mol/L hydrochloric acid solution, diluting and fixing the volume to scale to prepare a solution with the concentration of 100.0 mu g/m L;
weighing doxycycline reference substance 20.00mg, β -doxycycline reference substance 10.00mg, mettacycline reference substance 10.00mg and oxytetracycline reference substance 10.00mg, adding 0.01 mol/L hydrochloric acid solution for dissolving and diluting to prepare mixed solution containing oxytetracycline, methacycline, β -doxycycline 0.1mg and doxycycline 0.2mg in each 1m L;
(3) and (3) after 1 needle of the solution in the step (2) is respectively put in, continuously collecting 5 needles of doxycycline control solution, and finishing the detection process.
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| CN113237966A (en) * | 2021-04-08 | 2021-08-10 | 海南通用康力制药有限公司 | Quality detection method of doxycycline hydrochloride |
| CN116818948A (en) * | 2023-07-05 | 2023-09-29 | 河北威远药业有限公司 | Method for detecting related substances in doxycycline hydrochloride |
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| CN113237965A (en) * | 2021-04-08 | 2021-08-10 | 海南通用康力制药有限公司 | Method for detecting related substances of doxycycline hydrochloride for injection |
| CN113237966A (en) * | 2021-04-08 | 2021-08-10 | 海南通用康力制药有限公司 | Quality detection method of doxycycline hydrochloride |
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