阅读说明：本技术 泊沙康唑肠溶片含量分析方法 (Method for analyzing content of posaconazole enteric-coated tablets ) 是由 潘端锦 王金国 马一丹 于 2020-05-28 设计创作，主要内容包括：本发明涉及泊沙康唑肠溶片含量分析方法,包括以下步骤,稀释剂配制,流动相配制,对照品溶液配制,供试品溶液配制,通过液相色谱仪测量供试品溶液峰面积A<Sub>u</Sub>,测量对照品溶液峰面积n次,计算出平均值A<Sub>s</Sub>,根据公式<Image he="129" wi="624" file="DDA0002513866570000011.GIF" imgContent="drawing" imgFormat="GIF" orientation="portrait" inline="no"></Image>计算出供试品溶液中泊沙康唑的百分含量；有益效果是：通过以上分析方法测定,能准确测试泊沙康唑肠溶片中的含量,达到质量控制的目的。(The invention relates to a content analysis method of posaconazole enteric-coated tablets, which comprises the following steps of diluent preparation, mobile phase preparation, reference substance solution preparation, test solution preparation, and measurement of peak area A of the test solution through a liquid chromatograph u Measuring the peak area of the reference solution n times, and calculating the average value A s According to the formula Calculating the percentage content of posaconazole in the test solution; the beneficial effects are that: the above analysis method can accurately determineThe content of the posaconazole enteric-coated tablet is tested to achieve the purpose of quality control.)

1. The method for analyzing the content of the posaconazole enteric-coated tablets comprises the following steps:

preparing a diluent: weighing 800mL of methanol and 200mL of water, and uniformly mixing to obtain the methanol-water mixture;

preparing a buffer solution: weighing 1.74g of dipotassium phosphate, dissolving in 1L of water, mixing uniformly, adjusting the pH value to 6.0 +/-0.05 by using 30% phosphoric acid solution, and filtering through a 0.45-mum porous filter membrane to obtain the potassium phosphate-potassium mixed solution;

preparing a mobile phase: the volume ratio of the buffer solution to the acetonitrile is 3: 7, uniformly mixing to obtain the product;

preparing a reference substance solution: preparing a solution of posaconazole with the preparation concentration of C_STD；

Preparing a test solution: preparing a solution from the posaconazole enteric-coated tablets, and filtering the solution through a 0.45-micron porous filter membrane;

measuring the area A of the peak of posaconazole in the test solution by a liquid chromatograph_u，

Measurement of Posaconazole peak surface in control by liquid chromatographProduct A_S，

According to the formula

2. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 1, wherein: the diluent is prepared from methanol and water according to the weight ratio of 4: 1 proportion.

3. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 1, wherein: the phosphate used for preparing the buffer solution is a 30% phosphate solution.

4. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 3, wherein: the 30% phosphoric acid solution was diluted with 85% phosphoric acid.

5. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 1, wherein: the preparation method of the test solution comprises the following specific steps:

preparing a stock solution of a test sample: putting the posaconazole enteric-coated tablets into a volumetric flask, adding water, oscillating, adding methanol, and oscillating;

preparing a test solution: diluting the stock solution of the test sample, filtering with a filter membrane, discarding the initial filtrate, and collecting the subsequent filtrate.

6. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 1, wherein: the parameters of the liquid chromatograph are set to be 262nm of wavelength, 1.2mL/min of flow rate and 20 mu L of sample injection volume.

7. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 1, wherein: wherein Cs is the theoretical concentration of posaconazole in the test solution.

8. The method for analyzing the content of posaconazole enteric-coated tablets according to claim 1, wherein: the preparation method of the reference solution comprises the following specific steps:

preparing a reference substance stock solution: adding posaconazole into a volumetric flask, adding a diluent, and performing ultrasonic oscillation;

preparing a reference substance solution: and (4) taking the reference substance stock solution to a volumetric flask, and diluting.

Technical Field

The invention belongs to the technical field of medicine detection, and relates to an analysis method for content determination of posaconazole enteric-coated tablets.

Background

The posaconazole is a derivative of itraconazole, is a second-generation triazole antifungal drug, and is developed by American Moshadong pharmacy as an original product. The posaconazole enteric-coated tablets are listed in the first recommendation list of encouragement imitation drugs released by the country. At present, no inspection and analysis method for the product exists in Chinese pharmacopoeia.

Disclosure of Invention

In order to solve the problems, the invention adopts the following technical scheme:

the method for analyzing the content of the posaconazole enteric-coated tablets comprises the following steps:

preparing a diluent: mixing 800ml of methanol and 200ml of water uniformly to obtain the product;

preparing a buffer solution: adjusting the pH value of the phosphoric acid solution to 6.0 +/-0.05, and filtering the solution by using a 0.45-micron porous filter membrane;

preparing a mobile phase: and (3) mixing the prepared buffer solution with acetonitrile according to a volume ratio of 3: 7, uniformly mixing;

preparing a reference substance solution: preparing a solution of posaconazole with the preparation concentration of C_STD；

Preparing a test solution: preparing a solution from the posaconazole enteric-coated tablets, and filtering the solution by using a 0.45-micron porous filter membrane;

measuring the area A of the peak of posaconazole in the test solution by a liquid chromatograph_u，

Measuring the area A of the peak of posaconazole in a reference solution by a liquid chromatograph_S，

According to the formulaAnd calculating the content of the posaconazole in the test solution. (Cs is theoretical concentration of posaconazole in the test sample solution, and theoretical content calculation refers to the test sample bottle body composition table)

One way, the diluent is prepared from methanol and water according to a ratio of 4: 1, preparing the components in proportion;

in one mode, the phosphate used for preparing the buffer solution is a 30% phosphate solution;

in one mode, the 30% phosphoric acid solution is diluted with 85% phosphoric acid;

in one mode, the concrete steps of preparing the test solution are as follows:

preparing a stock solution of a test sample: putting the posaconazole enteric-coated tablets into a volumetric flask, adding water, oscillating, adding methanol, and oscillating;

preparing a test solution: diluting the stock solution of the test sample, filtering with a filter membrane, discarding the initial filtrate, and collecting the subsequent filtrate.

In one mode, the wavelength is 262nm, the flow rate is 1.2mL/min and the sample injection volume is 20 muL through the parameter setting of the liquid chromatograph.

In one embodiment, the preparation of the reference solution comprises the following steps:

preparing a reference substance stock solution: adding posaconazole into a measuring flask, adding a diluent, and performing ultrasonic oscillation;

preparing a reference substance solution: and (4) taking the reference substance stock solution to a volumetric flask, and diluting.

The invention has the beneficial effects that:

the content of the posaconazole enteric-coated tablet can be accurately tested by the determination of the analysis method, so that the purpose of quality control is achieved.

Detailed Description