CN-121994884-A - Method for quantitatively detecting 2,4, 6-trihydroxyacetophenone

Abstract

The invention relates to a method for quantitatively detecting 2,4, 6-trihydroxy acetophenone, which is characterized in that a 'K 2 S 2 O 8 -Na 2 S 2 O 3 -CuCl 2 -NH 4 OH' pH clock reaction system is used as a detection solution, and quantitative analysis of the 2,4, 6-trihydroxy acetophenone is realized according to different responses of the system to 2,4, 6-trihydroxy acetophenone with different concentrations, namely different induction times. The quantitative analysis method of the 2,4, 6-trihydroxy acetophenone has the characteristics of high accuracy, easy operation, convenience, quickness and the like.

Inventors

• HU GANG
• HU YONGJIE
• Duan Runqiu

Assignees

• 安徽大学

Dates

Publication Date

20260508

Application Date

20260131

Claims (3)

1. 1. A quantitative detection method of 2,4, 6-trihydroxyacetophenone is characterized in that: ethanol is used as a solvent to prepare a solution of the 2,4, 6-trihydroxyacetophenone of the sample to be detected; The method comprises the steps of using a 'K 2 S 2 O 8 -Na 2 S 2 O 3 - CuCl 2 -NH 4 OH' pH clock reaction system as a detection solution, recording a time-varying map of the pH of the clock system, controlling the temperature of the pH clock system to be within a range of 20-30 ℃, and adding equal volumes of serial sample solutions 2,4, 6-trihydroxyacetophenone to be detected with different concentrations into the pH clock system when the pH clock reaction starts, wherein the induction time generated by the system is different according to the different concentrations of the solution to be detected in the clock system, so as to realize quantitative detection of the sample to be detected, and the induction time is the time required from the start of the pH clock system reaction to the stabilization of the pH; Establishing a working curve according to the relation between the concentration of the 2,4, 6-trihydroxy acetophenone in the pH clock system and the induction time, wherein the abscissa is the concentration of the 2,4, 6-trihydroxy acetophenone in the pH clock system, and the ordinate is the induction time t, when the concentration of the 2,4, 6-trihydroxy acetophenone in the system is between 2.5X10 -4 mol/L and 7.5X10 -4 mol/L, the induction time t and the concentration of the 2,4, 6-trihydroxy acetophenone form a linear relation, so that the quantitative detection of the 2,4, 6-trihydroxy acetophenone in the sample is realized; the molar concentration range of each component in the detection solution is as follows ：K 2 S 2 O 8 0.0115-0.0135 mol/L、Na 2 S 2 O 3 0.0021-0.0041 mol/L、CuCl 2 0.00005-0.00025 mol/L 、NH 4 OH 0.0015-0.0035 mol/L.
2. 2. The quantitative determination method according to claim 1, wherein the molar concentration of each component in the detection solution is ：K 2 S 2 O 8 0.01225 mol/L、Na 2 S 2 O 3 0.002952 mol/L、CuCl 2 0.000125mol/L 、NH 4 OH 0.0025 mol/L.
3. 3. The method of quantitative determination according to claim 1, wherein the temperature of the pH clock system is controlled at 25℃when detecting the 2,4, 6-trihydroxyacetophenone solution.

Description

Method for quantitatively detecting 2,4, 6-trihydroxyacetophenone Technical Field The invention relates to an analysis and detection method, in particular to a method for establishing a K 2S2O8-Na2S2O3-CuCl2 -NH4 OH clock system, realizing quantitative analysis of 2,4, 6-trihydroxy acetophenone according to different responses of the system to 2,4, 6-trihydroxy acetophenone with different concentrations, namely different induction time, and belonging to the field of analytical chemistry. Background The 2,4, 6-trihydroxyacetophenone has a structure shown in formula (I), and is yellowish crystal or powder in appearance, and can be dissolved in ethanol, diethyl ether, chloroform, ethyl acetate and hot water. 2,4, 6-trihydroxy acetophenone is aglycone part of acetophenone glycoside in Curcuma longa, has cholesterol lowering effect, and can enhance activity of cholesterol 7α -hydroxylase, and 2,4, 6-trihydroxy acetophenone stimulates bile secretion via multi-drug resistance related protein 2. Therefore, the method is commonly used for medical intermediates, synthesizing novel antioxidant flavanone and the like. The current detection methods for the 2,4, 6-trihydroxyacetophenone comprise high performance liquid chromatography, ultraviolet-visible spectroscopy, nuclear magnetic resonance hydrogen spectrometry and the like. However, the methods have the defects of complex operation and higher cost, and the quantitative analysis method of the 2,4, 6-trihydroxyacetophenone has the characteristics of high accuracy, easy operation, convenience, quickness and the like. Structure of 2,4, 6-trihydroxyacetophenone of structural formula (I) Disclosure of Invention The invention aims to provide a novel quantitative detection method for 2,4, 6-trihydroxy acetophenone, namely a method for quantitatively detecting 2,4, 6-trihydroxy acetophenone by taking a 'K 2S2O8-Na2S2O3- CuCl2 -NH4 OH' pH clock system as a detection solution, and the method is a standard curve (working curve) method developed based on the sensitive response of the pH clock system to 2,4, 6-trihydroxy acetophenone. The method comprises the steps of using a 'K 2S2O8-Na2S2O3-CuCl2 -NH4 OH' pH clock reaction system as a detection solution, recording a pH time-varying map, respectively adding equal volumes of a series of 2,4, 6-trihydroxy acetophenone sample solutions to be detected with different concentrations into the pH clock system when the pH clock reaction starts, and quantitatively detecting the 2,4, 6-trihydroxy acetophenone sample according to different induction time generated by the system when the concentration of the solution to be detected in the pH clock system is different, wherein the induction time is the time required from the beginning of the pH clock system reaction to the stabilization of the pH; And establishing a working curve according to the relation between the concentration of 2,4, 6-trihydroxy acetophenone in the pH clock system and the induction time, wherein the abscissa is the concentration of 2,4, 6-trihydroxy acetophenone in the pH clock system, the ordinate is the induction time t, and when the concentration of 2,4, 6-trihydroxy acetophenone in the system is between 2.5X10 -4 mol/L and 7.5X10 -4 mol/L, the induction time t and the concentration of 2,4, 6-trihydroxy acetophenone form a linear relation, so that the quantitative detection of the 2,4, 6-trihydroxy acetophenone in the sample can be realized. The quantitative detection method is different from the prior art in that the method uses a 'K 2S2O8-Na2S2O3- CuCl2 -NH4 OH' pH clock system as a detection solution, and the system has different responses, namely different induction times, to 2,4, 6-trihydroxy acetophenone with different concentrations, so as to realize the quantitative analysis to the 2,4, 6-trihydroxy acetophenone. The concentration of 2,4, 6-trihydroxyacetophenone detected in the detection solution (pH clocking system) ranged from 2.5X10 -4 mol/L to 7.5X10 -4 mol/L. When 2,4, 6-trihydroxyacetophenone is detected in a detection solution (pH clock system), the pH clock system temperature is controlled at any one specific temperature within the range of 20-30 ℃. The concentration range in which 2,4, 6-trihydroxyacetophenone can be detected is the experimentally determined optimal concentration range using the above pH clock system. In the concentration range, the induction time has good response to the concentration change of the 2,4, 6-trihydroxy acetophenone, and the linear correlation coefficient is large. In addition, the concentration ranges of the components in the detection solution (pH clock system) are shown in table 1, and the optimal concentrations of the detection solution (pH clock system) obtained through a plurality of experiments are shown in table 2: TABLE 1 concentration ranges of the components in the pH clock System TABLE 2 optimal concentration of the components in the pH clock System The specific experimental steps are as follows: 1. Pr