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Method for analyzing substituent-containing naphthalene ring

An analytical method and technology of substituents, applied in the field of pharmaceutical analysis, can solve the problems of lack of quality control standards for compounds, and achieve the effect of good separation effect, simple analysis method and good peak shape.

Active Publication Date: 2020-10-02
天津汉一医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiencies in the prior art, the object of the present invention is to provide a method for analyzing the naphthalene ring containing substituents, so as to solve the problem that such compounds lack quality control standards

Method used

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  • Method for analyzing substituent-containing naphthalene ring
  • Method for analyzing substituent-containing naphthalene ring
  • Method for analyzing substituent-containing naphthalene ring

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In this embodiment, the following methods are used to analyze the naphthalene ring structure containing substituents:

[0033] (compound 1) and (compound 2).

[0034] Accurately weigh the appropriate amount of the above two compounds, put them in the same measuring bottle, add a mixed solvent of acetonitrile and water with a volume ratio of 50:50 to dissolve, and dilute to make about 0.5 mg of hydrochloric acid compound 2 and 0.5 mg of hydrochloric acid compound 1 in every 1 mL. , 5 μg and shake well.

[0035] The liquid chromatographic conditions of the analytical method are: the chromatographic column model is Chiralpak AY-RH, 150×4.6mm, 5 μm, the detection wavelength is 222 nm, the column temperature is 25°C, the flow rate is 0.4 mL / min, and the injection volume is 10 μL , the mobile phase is a mixed solution of ammonium bicarbonate aqueous solution and acetonitrile with a concentration of 20mmol / L, and the volume ratio is 50:50. The results are as follows figu...

Embodiment 2

[0039] The difference between this example and Example 1 is that the flow rate of this example is 0.5 mL / min, and the rest are analyzed the same as Example 1. The results showed that the resolution of compound 1 and compound 2 was 9.45.

Embodiment 3

[0041] The difference between this embodiment and Example 1 is that the concentration of the ammonium bicarbonate aqueous solution is 25 mmol / L, and all the others are analyzed the same as in Example 1. The results showed that the resolution of compound 1 and compound 2 was 9.67.

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Abstract

The invention provides an analysis method of a substituent-containing naphthalene ring. The liquid chromatography conditions of the analysis method are as follows: the model of the chromatographic column is Chiralpak AY-RH, 150*4.6mm, 5<mu>m; the detection wavelength is 220-230 nm, the column temperature is 22-28 DEG C, the flow rate is 0.2-0.5 mL / min, the sample injection amount is 10 <mu>L, themobile phase is a mixed solution of an ammonium bicarbonate aqueous solution and acetonitrile, and a solvent of the to-be-detected sample is a mixed solvent of acetonitrile and water. According to thepresent invention, the reversed phase chromatography condition is adopted, such that the separation degree of the substituent-containing naphthalene ring structure and the similar structure is improved under the conditions of the specific wavelength, the specific mobile phase and the specific flow rate, the separation degree can achieve more than or equal to 10, and compared to the existing method, the separation effect is good, the quality control of the actual production is easily achieved, and the good application prospect is provided.

Description

technical field [0001] The invention belongs to the field of drug analysis and relates to an analysis method for a naphthalene ring containing a substituent. Background technique [0002] Naphthalene rings containing substituents are an important class of pharmaceutical intermediates or can be used as a potential drug. How to establish a general detection method is of great value for this type of compound in drug analysis and quality control. [0003] At present, the analysis methods for such compounds mainly focus on the forward analysis, and the salts used in the mobile phase are mainly concentrated on phosphates such as potassium dihydrogen phosphate and sodium dihydrogen phosphate, and it has also been reported that diethylamine is used as the mobile phase. However, these analytical methods cannot fully meet the quality control requirements of such compounds at present, and it is urgent to develop a more general method with good separation effect between different substa...

Claims

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Application Information

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IPC IPC(8): G01N30/89G01N30/34
CPCG01N30/34G01N30/89
Inventor 严洁
Owner 天津汉一医药科技有限公司