Method for measuring content of auxiliary material cellulose in medicine by liquid phase technology

Abstract

The invention belongs to the technical field of pharmaceutical analysis, and provides a method for measuring the content of auxiliary material cellulose in a medicine by a liquid phase technology. The method comprises the following steps: respectively injecting a test solution and a reference solution into a liquid chromatograph, and measuring the content by adopting an electric fog type detector, wherein a chromatographic column of the liquid phase technology is a gel chromatographic column, a mobile phase A of the liquid phase technology is a salt solution, and a mobile phase B of the liquid phase technology is acetonitrile. Through specificity, linearity, repeatability, accuracy and stability verification, the method can be used for accurately measuring the content of cellulose in the medicine.

Description

technical field

[0001] The application belongs to the technical field of pharmaceutical analysis, and in particular relates to a liquid-phase method for determining the content of cellulose as an excipient in medicine. Background technique

[0002] Pharmaceutical excipients refer to the excipients and additives used in the production of drugs and the preparation of prescriptions. They are indispensable components of drugs and are closely related to drug quality and drug safety. Generally, pharmaceutical excipients have passed a reasonable assessment in terms of safety, but as a chemical component, they are not completely inert, and are especially affected by the matrix of pharmaceutical ingredients. Some excipients are not only active, but may also exhibit toxic reactions. Therefore, it is necessary to monitor the content of pharmaceutical excipients.

[0003] Cellulose is a kind of macromolecular polysaccharide composed of glucose. Due to its wide range of sources and uniq...

Examples

Embodiment 1

[0032] The method for determining the cellulose content of the auxiliary material in the liquid phase method comprises the steps:

[0033] 1. Liquid chromatography conditions: Chromatographic column: TSKgtl G2000SW column, 60cm*7.5mm, 10μm; detector: charged aerosol detector; mobile phase: 10mmol / L ammonium acetate solution (pH 4.5): acetonitrile=95:5; Atomization temperature: 50°C; flow rate: 1.0ml / min; injection volume: 10μl.

[0034] 2. Reference substance solution: Accurately weigh 25.79 mg of hydroxyethyl cellulose reference substance, accurately weigh it, put it in a 50ml measuring bottle, add warm water (60°C) to dissolve it, add water to dilute to the mark, and shake well to obtain hydroxyethyl cellulose Ethyl cellulose reference substance stock solution. Then precisely pipette 5ml of the hydroxyethyl cellulose reference substance stock solution into a 10ml volumetric flask, dilute with water to the mark, and shake well to obtain the reference substance solution.

[...

Embodiment 2

[0039] The method for the determination of the cellulose content of excipients in drugs by liquid phase method was validated, and the validation results are as follows:

[0040] 1. Specificity: Get solvent water, reference substance solution, negative blank solution, need testing solution and standard-added need testing solution respectively and detect by the chromatographic conditions of embodiment 1, record chromatogram, investigate method specificity.

[0041] see results Figure 1~2 Shown, blank solution and negative blank solution ( figure 2 ) did not detect the target peak, no interference to the detection; the reference substance solution showed the target peak, and no other impurity peaks were detected ( figure 1 ); the test solution ( image 3 ) and the retention time of the target peak in the chromatogram of the standard-added test solution is consistent with the retention time of the main peak in the reference solution (retention time is between 10.483min~10.515m...

Embodiment 3

[0058] Detect reference substance solution and need testing solution respectively with reference to the method condition of embodiment, difference only is to adjust the pH of ammonium acetate solution to be 4.3 and 4.7, record chromatogram, calculate the hydroxyethyl cellulose concentration in reference substance solution and need testing solution Get the content. The results showed that the pH value of the mobile phase fluctuated in the range of 4.3-4.7, the RSD of the peak area of ​​hydroxyethyl cellulose in the reference solution for 6 consecutive times was between 0.4% and 2.1%, and the RSD of the retention time was between 0.2 and 0.4%. The RSD of the hydroxyethyl cellulose content measured in the test solution was 2.7%, and the durability result met the requirements.

technical field

[0001] The application belongs to the technical field of pharmaceutical analysis, and in particular relates to a liquid-phase method for determining the content of cellulose as an excipient in medicine. Background technique

[0002] Pharmaceutical excipients refer to the excipients and additives used in the production of drugs and the preparation of prescriptions. They are indispensable components of drugs and are closely related to drug quality and drug safety. Generally, pharmaceutical excipients have passed a reasonable assessment in terms of safety, but as a chemical component, they are not completely inert, and are especially affected by the matrix of pharmaceutical ingredients. Some excipients are not only active, but may also exhibit toxic reactions. Therefore, it is necessary to monitor the content of pharmaceutical excipients.

[0003] Cellulose is a kind of macromolecular polysaccharide composed of glucose. Due to its wide range of sources and uniq...

Examples

Embodiment 1

[0032] The method for determining the cellulose content of the auxiliary material in the liquid phase method comprises the steps:

[0033] 1. Liquid chromatography conditions: Chromatographic column: TSKgtl G2000SW column, 60cm*7.5mm, 10μm; detector: charged aerosol detector; mobile phase: 10mmol / L ammonium acetate solution (pH 4.5): acetonitrile=95:5; Atomization temperature: 50°C; flow rate: 1.0ml / min; injection volume: 10μl.

[0034] 2. Reference substance solution: Accurately weigh 25.79 mg of hydroxyethyl cellulose reference substance, accurately weigh it, put it in a 50ml measuring bottle, add warm water (60°C) to dissolve it, add water to dilute to the mark, and shake well to obtain hydroxyethyl cellulose Ethyl cellulose reference substance stock solution. Then precisely pipette 5ml of the hydroxyethyl cellulose reference substance stock solution into a 10ml volumetric flask, dilute with water to the mark, and shake well to obtain the reference substance solution.

[...

Embodiment 2

[0039] The method for the determination of the cellulose content of excipients in drugs by liquid phase method was validated, and the validation results are as follows:

[0040] 1. Specificity: Get solvent water, reference substance solution, negative blank solution, need testing solution and standard-added need testing solution respectively and detect by the chromatographic conditions of embodiment 1, record chromatogram, investigate method specificity.

[0041] see results Figure 1~2 Shown, blank solution and negative blank solution ( figure 2 ) did not detect the target peak, no interference to the detection; the reference substance solution showed the target peak, and no other impurity peaks were detected ( figure 1 ); the test solution ( image 3 ) and the retention time of the target peak in the chromatogram of the standard-added test solution is consistent with the retention time of the main peak in the reference solution (retention time is between 10.483min~10.515m...

Embodiment 3

[0058] Detect reference substance solution and need testing solution respectively with reference to the method condition of embodiment, difference only is to adjust the pH of ammonium acetate solution to be 4.3 and 4.7, record chromatogram, calculate the hydroxyethyl cellulose concentration in reference substance solution and need testing solution Get the content. The results showed that the pH value of the mobile phase fluctuated in the range of 4.3-4.7, the RSD of the peak area of ​​hydroxyethyl cellulose in the reference solution for 6 consecutive times was between 0.4% and 2.1%, and the RSD of the retention time was between 0.2 and 0.4%. The RSD of the hydroxyethyl cellulose content measured in the test solution was 2.7%, and the durability result met the requirements.

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