Method for detecting content of polymer in cefuroxime sodium medicine

Abstract

The invention discloses a method for detecting the content of a polymer in a cefuroxime sodium medicine, and relates to the technical field of detection of the content of the polymer in the medicine, the method for detecting the content of the polymer in the cefuroxime sodium medicine comprises the following operation steps: S1, setting chromatographic conditions; s2, preparing a solution; s3, obtaining a chromatogram map; and S4, calculating the content of the polymer. According to the method for detecting the content of the polymer in the cefuroxime sodium medicine, the content of the polymer in the cefuroxime sodium medicine is accurately determined by matching a main component external standard method with a mobile phase, namely an aqueous solution as a blank reagent, a test solution and a contrast solution, and the detection time is greatly shortened on the basis of the accuracy of a detection result.

Description

Technical Field

[0001] The present invention relates to the technical field of detecting the polymer content in drugs, and specifically to a method for detecting the polymer content in cefuroxime sodium drugs. Background Art

[0002] In the antibiotic market, cephalosporin antibiotics occupy a large share, including cefmetazole sodium, ceftriaxone sodium, cefuroxime sodium, etc., which belong to the second-generation and third-generation cephalosporin antibiotics respectively. Cephalosporin antibiotics can form high-molecular polymers, which cause immediate allergic reactions in clinical use and pose great harm to patients. Therefore, it is necessary to detect the polymer content in cephalosporin drugs.

[0003] At present, the 2020 edition of the Chinese Pharmacopoeia includes detection methods for high-molecular polymers in more than 10 cephalosporin antibiotic drug raw materials and their preparations, and basically adopts the traditional molecular exclusion chromatography method. However, the molecular exclusion chromatography method is inaccurate in determining the polymer content in cephalosporin antibiotic drugs and has a long detection cycle.

[0004] Therefore, in view of this, research and improvement are carried out on the existing structure and deficiencies, and a method for detecting the polymer content in cefuroxime sodium drugs is proposed. Summary of the Invention

[0005] In view of the deficiencies of the prior art, the present invention provides a method for detecting the polymer content in cefuroxime sodium drugs, and solves the problems raised in the above background art.

[0006] To achieve the above objectives, the present invention is realized through the following technical solutions: A method for detecting the polymer content in cefuroxime sodium drugs, the method for detecting the polymer content in cefuroxime sodium drugs includes the following operating steps:

[0007] S1. Chromatographic conditions:

[0008] Chromatographic column: Welch Utimate LP-C8 4.6X250mm 5μm;

[0009] Flow rate: 1.5 ml / min;

[0010] Detector: Ultraviolet-visible spectrophotometric detector;

[0011] Detection wavelength: 273 nm;

[0012] Column temperature: 30°C;

[0013] Injection volume: 10 μl;

[0014] Mobile phase: Aqueous solution;

[0015] S2. Solution preparation:

[0016] Prepare the test solution and the control solution. The test solution is a solution containing cefuroxime sodium, and the control solution is a dilution of the test solution.

[0017] S3. Chromatogram:

[0018] Detect the test solution and the control solution to obtain the chromatogram of the test solution and the chromatogram of the control solution.

[0019] S4. Calculate the polymer content:

[0020] According to the chromatograms of the test solution and the control solution, use the external standard method of the main component to calculate the content of the polymer in cefuroxime sodium.

[0021] Furthermore, in the step S1, the preparation process of the aqueous solution is as follows:

[0022] Weigh 0.385 g of ammonium acetate into 1 L of water, dissolve and mix well, adjust the pH to 3.4 with glacial acetic acid to obtain the initial solution. Then take the above initial solution and mix it evenly with acetonitrile in a ratio of 70:30. After mixing evenly, filter it through a 0.45-μm filter membrane and perform ultrasonic degassing to obtain the aqueous solution.

[0023] Furthermore, in the step S2, the preparation process of the control solution is as follows:

[0024] Weigh cefuroxime sodium, dissolve it in water after weighing, and quantitatively dilute it to a solution containing 170 μg of cefuroxime sodium per 1 ml.

[0025] Furthermore, in the step S3, the high performance liquid chromatography method is used when detecting the test solution and the control solution.

[0026] Furthermore, in the step S3, the chromatographic conditions in the step S1 are used when obtaining the chromatograms of the test solution and the control solution.

[0027] Furthermore, in the step S4, the external standard method of the main component means adding a certain amount of reference substance to the blank solvent according to the gradient to prepare a reference sample, that is, the control solution, and performing sample treatment and detection in parallel with the unknown sample, that is, the test solution. Inject the reference substances with different concentrations, plot a standard curve with the peak area as the value, and thus calculate the concentration of the measured component in the unknown sample.

[0028] Furthermore, in the step S4, the calculation formula of the external standard method of the main component is as follows:

[0029] (cx) = cr * Ax / Ar.

[0030] Further, (cx) is the sample concentration, i.e., the polymer content of the test substance, cr is the concentration of the control solution, Ax is the sample peak area, and Ar is the control peak area.

[0031] Further, the method for detecting the polymer content in cefuroxime sodium drug is used to detect the polymer content in cefuroxime sodium drug.

[0032] The present invention provides a method for detecting the polymer content in cefuroxime sodium drug, which has the following beneficial effects:

[0033] 1. The method for detecting the polymer content in cefuroxime sodium drug can accurately determine the polymer content in cefuroxime sodium drug by the external standard method of the main component in combination with the mobile phase: aqueous solution as the blank reagent, the test solution and the control solution, and greatly shorten the detection time on the basis of the accuracy of the detection result. Description of the Drawings

[0034] Figure 1 It is a schematic flow chart of the operation steps of the method for detecting the polymer content in cefuroxime sodium drug of the present invention. Detailed Embodiments

[0035] The following further describes the embodiments of the present invention in detail with reference to the drawings and examples. The following examples are used to illustrate the present invention, but cannot be used to limit the scope of the present invention.

[0036] As Figure 1 shown, the present invention provides a technical solution: a method for detecting the polymer content in cefuroxime sodium drug, and the method for detecting the polymer content in cefuroxime sodium drug includes the following operation steps:

[0037] S1. Chromatographic conditions:

[0038] Chromatographic column: Welch Utimate LP-C8 4.6X250mm 5μm;

[0039] Flow rate: 1.5 ml / min;

[0040] Detector: Ultraviolet-visible spectrophotometric detector;

[0041] Detection wavelength: 273 nm;

[0042] Column temperature: 30 °C;

[0043] Injection volume: 10 μl;

[0044] Mobile phase: aqueous solution, and the preparation process of the aqueous solution is as follows:

[0045] Weigh 0.385 g of ammonium acetate and dissolve it in 1 L of water. Mix it evenly in a mixing device. After mixing, adjust it with glacial acetic acid and inject it into the mixing device at a flow rate of 1.0 - 10.0 ml / s until the pH of the mixed solution is adjusted to 3.4 to obtain the initial solution. Then, take the above initial solution and mix it evenly with acetonitrile in a ratio of 70:30. After mixing evenly, filter it through a 0.45-μm filter membrane and degas it by ultrasonic treatment to obtain the aqueous solution;

[0046] Among them, the mobile phase: the aqueous solution also serves as a blank reagent;

[0047] S2. Solution preparation:

[0048] Prepare the test solution and the control solution. The test solution is a solution containing cefuroxime sodium drug, and the control solution is a dilution of the test solution;

[0049] The preparation process of the control solution is as follows:

[0050] Weigh cefuroxime sodium drug, dissolve it in water and quantitatively dilute it to a solution containing 170 μg of cefuroxime sodium per 1 ml;

[0051] S3. Chromatogram:

[0052] Detect the test solution and the control solution to obtain the chromatogram of the test solution and the chromatogram of the control solution. Among them, when detecting the test solution and the control solution, the high-performance liquid chromatography method is used, and when obtaining the chromatograms of the test solution and the control solution, the chromatographic conditions in step S1 are adopted;

[0053] S4. Calculate the polymer content:

[0054] According to the chromatograms of the test solution and the control solution, use the external standard method of the main component to calculate the content of the polymer in the cefuroxime sodium drug;

[0055] The external standard method of the main component means adding a certain amount of reference substance to the blank solvent according to the gradient to prepare a reference sample, that is, the control solution, and performing sample treatment and detection in parallel with the unknown sample, that is, the test solution. Inject the reference substances with different concentrations, plot a standard curve with the peak area as the value, and thus calculate the concentration of the measured component in the unknown sample;

[0056] The calculation formula of the external standard method of the main component is as follows:

[0057] (cx) = cr * Ax / Ar, where (cx) is the sample concentration, that is, the polymer content of the test solution, cr is the concentration of the control solution, Ax is the sample peak area, and Ar is the reference peak area;

[0058] The method for detecting the content of polymers in cefuroxime sodium drug accurately determines the content of polymers in cefuroxime sodium drug by using the external standard method for the main component in combination with the mobile phase: aqueous solution as the blank reagent, the test solution and the reference solution, and greatly shortens the detection time based on the accuracy of the detection results;

[0059] The method for detecting the content of polymers in cefuroxime sodium drug is used to detect the content of polymers in cefuroxime sodium drug.

[0060] In summary, as Figure 1 shown, when using the method for detecting the content of polymers in cefuroxime sodium drug, first prepare the test solution and the reference solution. The test solution is a solution containing cefuroxime sodium drug, and the reference solution is a dilution of the test solution; the preparation process of the reference solution is as follows:

[0061] Weigh cefuroxime sodium drug, dissolve it in water and quantitatively dilute it to a solution containing 170 μg of cefuroxime sodium per 1 ml;

[0062] Detect the test solution and the reference solution to obtain the chromatogram of the test solution and the chromatogram of the reference solution. Among them, when detecting the test solution and the reference solution, high performance liquid chromatography is used, and the chromatographic conditions for obtaining the chromatograms of the test solution and the reference solution are as follows:

[0063] Chromatographic column: Welch Utimate LP-C8 4.6X250mm 5μm;

[0064] Flow rate: 1.5 ml / min;

[0065] Detector: ultraviolet-visible spectrophotometric detector;

[0066] Detection wavelength: 273 nm;

[0067] Column temperature: 30 °C;

[0068] Injection volume: 10 μl;

[0069] Mobile phase: aqueous solution. Among them, the preparation process of the aqueous solution is as follows:

[0070] Weigh 0.385 g of ammonium acetate into 1 L of water, dissolve and mix well in a mixing device. After mixing, adjust with glacial acetic acid and inject into the mixing device at a flow rate of 1.0 - 10.0 ml / s until the pH of the mixed solution is adjusted to 3.4 to obtain the initial solution. Then take the above initial solution and mix it evenly with acetonitrile in a ratio of 70:30. After mixing evenly, filter it with a 0.45 μm filter membrane and ultrasonically degas to obtain the aqueous solution;

[0071] Among them, the mobile phase: aqueous solution also serves as the blank reagent;

[0072] Based on the chromatograms of the test solution and the reference solution, the content of polymers in cefuroxime sodium drug is calculated by the external standard method of the main component; the external standard method of the main component means that a certain amount of reference substance is added in gradient to the blank solvent to prepare a reference sample, that is, the reference solution, and the sample treatment and detection are carried out in parallel with the unknown sample, that is, the test solution. The reference substances with different concentrations are injected, and a standard curve is drawn with the peak area as the value, so as to calculate the concentration of the component to be measured in the unknown sample.

[0073] The calculation formula of the external standard method of the main component is as follows:

[0074] (cx) = cr * Ax / Ar, where (cx) is the sample concentration, that is, the polymer content of the test solution, cr is the concentration of the reference solution, Ax is the sample peak area, and Ar is the reference peak area;

[0075] Based on the external standard method of the main component, the content of polymers in cefuroxime sodium drug is calculated.

[0076] The embodiments of the present invention are given for the purpose of illustration and description, and are not exhaustive or limit the present invention to the disclosed form. Many modifications and variations are obvious to those of ordinary skill in the art. The embodiments are selected and described to better illustrate the principles and practical applications of the present invention, and enable those of ordinary skill in the art to understand the present invention and thus design various embodiments with various modifications suitable for specific purposes.

Claims

1. A method for detecting the content of polymers in cefuroxime sodium, characterized in that: The method for detecting the content of polymer in cefuroxime sodium drug comprises the following operating steps: S1. Chromatographic conditions: Chromatographic column: Welch Utimate LP-C8 4.6X250mm 5μm; Flow rate: 1.5 ml / min; Detector: ultraviolet-visible spectrophotometric detector; Detection wavelength: 273 nm; Column temperature: 30 °C; Injection volume: 10 μl; Mobile phase: aqueous solution; S2. Solution preparation: Prepare a test solution and a control solution. The test solution is a solution containing cefuroxime sodium drug, and the control solution is a dilution of the test solution; S3. Chromatogram: Detect the test solution and the control solution to obtain the chromatogram of the test solution and the chromatogram of the control solution; S4. Calculate the polymer content: According to the chromatograms of the test solution and the control solution, adopt the external standard method of the main component to calculate the content of polymer in cefuroxime sodium drug.

2. The method for detecting the content of polymer in cefuroxime sodium drug according to claim 1, wherein: In the step S1, the preparation process of the aqueous solution is as follows: Weigh 0.385 g of ammonium acetate into 1 L of water, dissolve and mix evenly, adjust the pH to 3.4 with glacial acetic acid as the initial solution, then take the above initial solution and acetonitrile and mix them evenly in a ratio of 70:

30. After mixing evenly, filter with a 0.45 μm filter membrane and perform ultrasonic degassing to obtain the aqueous solution.

3. The method for detecting the content of polymers in cefuroxime sodium drug according to claim 1, characterized in that: In the step S2, the preparation process of the control solution is as follows: Weigh cefuroxime sodium drug, dissolve it in water and quantitatively dilute it to a solution containing 170 μg of cefuroxime sodium per 1 ml.

4. The method for detecting the content of polymers in cefuroxime sodium drug according to claim 1, characterized in that: In the step S3, the high performance liquid chromatography method is adopted when detecting the test solution and the control solution.

5. The method for detecting the content of polymers in cefuroxime sodium drug according to claim 1, characterized in that: In the step S3, the chromatographic conditions in the step S1 are adopted when obtaining the chromatograms of the test solution and the control solution.

6. The method for detecting the content of polymers in cefuroxime sodium drug according to claim 1, wherein: In the step S4, the external standard method of the main component means adding a certain amount of reference substance to the blank solvent according to the gradient to prepare a reference sample, that is, the control solution, and performing sample treatment and detection in parallel with the unknown sample, that is, the test solution. Inject different concentrations of the reference substance, plot a standard curve with the peak area as the value, and thus calculate the concentration of the measured component in the unknown sample.

7. The method for detecting the content of polymer in cefuroxime sodium drug according to claim 1, wherein: In the step S4, the calculation formula of the external standard method of the main component is as follows: (cx) = cr * Ax / Ar.

8. The method for detecting the content of polymer in cefuroxime sodium drug according to claim 7, characterized in that: The (cx) is the sample concentration, that is, the polymer content of the test solution, cr is the concentration of the control solution, Ax is the sample peak area, and Ar is the control peak area.

9. The method for detecting the content of polymer in cefuroxime sodium drug according to any one of claims 1-8, characterized in that: The method for detecting the content of polymer in cefuroxime sodium drug is used to detect the content of polymer in cefuroxime sodium drug.

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