阅读说明：本技术 硝酸咪康唑的含量检测方法 (Method for detecting content of miconazole nitrate ) 是由 徐奇清 孙迎 聂姣 叶小妹 赵奉君 于 2018-07-23 设计创作，主要内容包括：本发明涉及一种硝酸咪康唑的含量检测方法,用溶剂将待测样品稀释成硝酸咪康唑的含量为0.02mg/mL～0.2mg/mL的供试品溶液；取10μL～20μL所述供试品溶液注入高效液相色谱仪中进行检测,得到所述待测样品中硝酸咪康唑的含量；所述高效液相色谱检测时的色谱条件为：色谱柱：以十八烷基硅烷键合硅胶为填充剂；流动相：由乙腈、磷酸盐溶液和三乙胺按体积比为(35～50):(50～65):1组成,所述流动相的pH值为3±0.1,所述磷酸盐溶液的浓度为0.02mol/L～0.08mol/L；流速：0.5mL/min～1.5mL/min；柱温：25℃～35℃；检测波长：210nm～240nm；所述溶剂的组成与所述流动相相同。该方法条件响应值高,硝酸咪康唑出峰快,能够实现快速测定其含量,提高了检测工作效率,有利于控制产品的质量。(The invention relates to a method for detecting the content of miconazole nitrate, which comprises the following steps of diluting a sample to be detected into a sample solution with the content of miconazole nitrate of 0.02 mg/mL-0.2 mg/mL by using a solvent; injecting 10-20 mu L of the sample solution into a high performance liquid chromatograph for detection to obtain the content of miconazole nitrate in the sample to be detected; the chromatographic conditions in the high performance liquid chromatography detection are as follows: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: the mobile phase consists of acetonitrile, phosphate solution and triethylamine according to the volume ratio of (35-50): (50-65): 1, the pH value of the mobile phase is 3 +/-0.1, and the concentration of the phosphate solution is 0.02 mol/L-0.08 mol/L; flow rate: 0.5mL/min to 1.5 mL/min; column temperature: 25-35 ℃; detection wavelength: 210nm to 240 nm; the solvent is of the same composition as the mobile phase. The method has high condition response value and quick miconazole nitrate peak emergence, can realize quick determination of the content of the miconazole nitrate peak, improves the detection working efficiency and is beneficial to controlling the quality of products.)

1. A method for detecting the content of miconazole nitrate is characterized by comprising the following steps:

diluting a sample to be detected into a sample solution to be detected with a solvent, wherein the content of miconazole nitrate is 0.02 mg/mL-0.2 mg/mL;

injecting 10-20 mu L of the sample solution into a high performance liquid chromatograph for detection to obtain the content of miconazole nitrate in the sample to be detected;

the chromatographic conditions in the high performance liquid chromatography detection are as follows:

a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent;

mobile phase: the mobile phase consists of acetonitrile, phosphate solution and triethylamine according to the volume ratio of (35-50): 50-65): 1, and the pH value of the mobile phase is 3 +/-0.1; the concentration of the phosphate solution is 0.02 mol/L-0.08 mol/L;

flow rate: 0.5mL/min to 1.5 mL/min;

column temperature: 25-35 ℃;

detection wavelength: 210nm to 240 nm;

the solvent is of the same composition as the mobile phase.

2. The method for detecting the content of miconazole nitrate according to claim 1, wherein the sample to be detected is shampoo containing miconazole nitrate.

3. The method for detecting the content of miconazole nitrate according to claim 1, wherein the mobile phase consists of acetonitrile, a phosphate solution and triethylamine in a volume ratio of (40-50): (50-60): 1.

4. The method for detecting the content of miconazole nitrate according to claim 3, wherein the mobile phase consists of acetonitrile, a phosphate solution and triethylamine in a volume ratio of 45:55: 1.

5. The method for detecting the content of miconazole nitrate according to claim 1, wherein the phosphate solution is a disodium hydrogen phosphate solution.

6. The method for detecting the content of miconazole nitrate according to claim 1, wherein the chromatographic column is ZORBZX Eclipse XDB-C18Analytical 4.6X 150mm 5-Micron or Kromasil 100-5-C184.6X 150 mm.

7. The method for detecting the content of miconazole nitrate according to claim 6, wherein the flow rate is 0.8mL/min to 1.2 mL/min.

8. The method for detecting the content of miconazole nitrate according to claim 1, wherein the content of miconazole nitrate in the sample solution is 0.05mg/mL to 0.15 mg/mL.

9. The method for detecting the content of miconazole nitrate according to any one of claims 1 to 8, wherein the regulator used for regulating the pH value of the mobile phase is phosphoric acid.

10. The method for detecting the content of miconazole nitrate according to any one of claims 1 to 8, wherein the method further comprises the following steps:

and performing HPLC detection on the miconazole nitrate reference substance according to an external standard method to obtain the relation between the content of the miconazole nitrate and the peak area, and calculating to obtain the content of the miconazole nitrate in the sample to be detected according to the relation between the content of the miconazole nitrate and the peak area of the miconazole nitrate in a chromatogram obtained by detecting the sample solution in a high performance liquid chromatograph.

Technical Field

The invention relates to the technical field of chemical detection, in particular to a method for detecting the content of miconazole nitrate.

Background

The shampoo is a transliteration of the foreign language 'shampoo', mainly comprises a detergent, an auxiliary detergent and an additive, and mainly has the effects of cleaning and caring hair; the additive can meet the special requirements of the shampoo and endow the shampoo with various different effects, so that the effect of the shampoo is continuously refined, and the compound shampoo preparation prepared by adding the medical components such as miconazole nitrate with antibacterial effect into the shampoo is a novel veterinary medicine shampoo preparation for pets.

The content detection method of the miconazole nitrate adopts a potentiometric titration method to determine, and the titration solution is usually 0.1mol/L perchloric acid titration solution; the potentiometric titration method is a method for determining a titration end point by measuring potential change in a titration process, has certain limitations in application, the sensitivity of the method may influence the accuracy of a detection result when detecting a low-concentration drug, perchloric acid is an inorganic acid with strong acidity, has strong oxidizing property, is easily decomposed at room temperature, has unstable factors as a titration solution, and the change of concentration easily causes errors in the detection result. In the Chinese pharmacopoeia, High Performance Liquid Chromatography (HPLC) is adopted to control only related substances in miconazole nitrate raw materials or single preparations thereof, and a detection method of a compound preparation thereof is not described. The experimental verification that the content of miconazole nitrate in the compound shampoo preparation is measured by adopting the method proves that the traditional method is not suitable for the content measurement of miconazole nitrate in the compound shampoo preparation. Therefore, at present, no effective method for the quality standard of the compound shampoo preparation and the detection of the content of miconazole nitrate exists.

Disclosure of Invention

Based on the detection method, the content of the miconazole nitrate in the shampoo containing the miconazole nitrate can be quickly and effectively detected.

A method for detecting the content of miconazole nitrate comprises the following steps:

diluting a sample to be detected into a sample solution to be detected with a solvent, wherein the content of miconazole nitrate is 0.02 mg/mL-0.2 mg/mL;

injecting 10-20 mu L of the sample solution into a high performance liquid chromatograph for detection to obtain the content of miconazole nitrate in the sample to be detected;

the chromatographic conditions in the high performance liquid chromatography detection are as follows:

a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent;

mobile phase: the mobile phase consists of acetonitrile, phosphate solution and triethylamine according to the volume ratio of (35-50): 50-65): 1, and the pH value of the mobile phase is 3 +/-0.1; the concentration of the phosphate solution is 0.02 mol/L-0.08 mol/L;

flow rate: 0.5mL/min to 1.5 mL/min;

column temperature: 25-35 ℃;

detection wavelength: 210nm to 240 nm;

the solvent is of the same composition as the mobile phase.

The miconazole nitrate content is not limited to mg/mL, and may be in other concentration units such as mass percentage content and molar concentration.

In one embodiment, the sample to be tested is shampoo containing miconazole nitrate.

In one embodiment, the detection wavelength is 226 nm.

In one embodiment, the mobile phase consists of acetonitrile, phosphate solution and triethylamine according to the volume ratio of (40-50): (50-60): 1.

In one embodiment, the mobile phase consists of acetonitrile, phosphate solution and triethylamine in a volume ratio of 45:55: 1.

In one embodiment, the phosphate solution is a disodium hydrogen phosphate solution.

Further, the concentration of the disodium hydrogen phosphate solution is 0.05 mol/L.

In one embodiment, the column is ZORBZX Eclipse XDB-C18Analytical 4.6X 150mm 5-Micron or Kromasil 100-5-C184.6X 150 mm.

Preferably, the column is ZORBZX Eclipse XDB-C18Analytical 4.6X 150mm 5-Micron.

In one embodiment, the flow rate is 0.8mL/min to 1.2 mL/min.

In one embodiment, the content of miconazole nitrate in the sample solution is 0.05 mg/mL-0.15 mg/mL.

In one embodiment, the adjusting agent used to adjust the pH of the mobile phase is phosphoric acid.

In one embodiment, the detection method further comprises the following steps:

and performing HPLC detection on the miconazole nitrate reference substance according to an external standard method to obtain the relation between the content of the miconazole nitrate and the peak area, and calculating to obtain the content of the miconazole nitrate in the sample to be detected according to the relation between the content of the miconazole nitrate and the peak area of the miconazole nitrate in a chromatogram obtained by detecting the sample solution in a high performance liquid chromatograph.

In one embodiment, a standard curve is drawn by using a miconazole nitrate reference substance according to an external standard method, and the content of miconazole nitrate in the sample to be detected is calculated according to the standard curve.

Specifically, a proper amount of miconazole nitrate reference substance is taken and prepared into a miconazole nitrate reference sample containing 0.02 mg/mL-0.2 mg/mL in the solvent, sample treatment and detection are carried out in parallel with the sample solution, the concentration of miconazole nitrate corresponding to each peak area is measured, and a standard curve is drawn;

and measuring the peak area of the miconazole nitrate in the chromatogram obtained by injecting the test solution into a high performance liquid chromatograph for detection, and calculating to obtain the content of the miconazole nitrate in the sample to be detected according to the standard curve.

According to the detection method, the appropriate mobile phase component is selected, the proportion composition of the mobile phase is adjusted, and other parameter conditions are combined, so that the response value of the detection condition is high, the miconazole nitrate peaks quickly under the condition that the component separation degree is ensured, the retention time of the miconazole nitrate can be effectively shortened, the content of the miconazole nitrate in a shampoo preparation containing the miconazole nitrate is quickly and accurately determined, the problem of determining the content of the miconazole nitrate in compound miconazole nitrate shampoo is solved, the detection work efficiency is greatly improved, and the quality of a product is favorably controlled. In addition, the detection method can be applied to shampoo preparations containing miconazole nitrate and can also be applied to content detection of miconazole nitrate in other products or preparations.

Drawings

FIG. 1 is HPLC detection spectrum of miconazole nitrate in compound miconazole nitrate shampoo of example 1;

FIG. 2 is the HPLC detection spectrum of miconazole nitrate control in example 1.

Detailed Description

In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The compound miconazole nitrate shampoo is self-made by Australian dragons pharmaceutical Co., Ltd, south China sea, mountain, and mainly comprises miconazole nitrate, a detergent, various additives and the like; miconazole nitrate controls were purchased from Sigma; acetonitrile and triethylamine were chromatographically pure, and disodium hydrogen phosphate and phosphoric acid were analytically pure.