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Method for measuring isomer impurities in p-fluorothiophenol by HPLC method

A technology of p-fluorothiophenol and fluorothiophenol, which is applied in the chemical and pharmaceutical fields, can solve problems such as unreported detection methods, and achieve the effects of high accuracy, strong specificity, and easy operation

Active Publication Date: 2021-10-26
连云港杰瑞药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there is no report on the detection method of isomer impurities in p-fluorothiophenol. Therefore, it is necessary to develop a method that can effectively detect isomer impurities in p-fluorothiophenol HPLC method for impurities is very necessary

Method used

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  • Method for measuring isomer impurities in p-fluorothiophenol by HPLC method
  • Method for measuring isomer impurities in p-fluorothiophenol by HPLC method
  • Method for measuring isomer impurities in p-fluorothiophenol by HPLC method

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Embodiment 1

[0051] Systematic precision and exclusive investigation:

[0052] Method for detecting amphiberic impurities in fluorine phenol in HPLC method, including the following steps: Instruments and chromatography conditions, instruments: high performance liquid chromatograph; column: ACE EXCEL C18-PFP, 4.6mm × 250mm, 5μm ; Liquid phase: 0.05% trifluoroacetic acid aqueous solution - methanol (50:50), wavelength: 238 nm, column temperature: 35 ° C, flow rate: 1.0ml / min, injection volume: 20μL, equal degree elution, recording chromatogram The main peak retention time is 2 times.

[0053] First, the solution is prepared, each impurities are positioned: precipitated with 1.0 ml of the impurity reserve, separately 50mL volumetric flask, add 2 ml of TCEP solution, shake, and dilute with methanol to the scale.

[0054] Precision amount takes a blank solution, the systematic solution, the reaction solution, each impurity positioning solution 20 μl, injects the liquid chromatography, and recordi...

Embodiment 2

[0056] Quantitative examination:

[0057]Precision mining impurities reserves the solution, add 2 ml of TCEP solution, dissolved and diluted with each impurity concentration of about 0.05 μg / ml, as a quantitative solvent. Cake 20 μl of the amount, continuous injection 6 times, record the chromatogram, the specific results are shown in Figure 3, each impurities quantitative limit measurement result, each impurities quantitative limit concentration and the tested product concentration ratio of 0.005%, 6 parts quantitative solution The RSD of the peak area is 8.1%, less than 10%. The detection sensitivity of benzene thiodol, 2-fluorophenol, and 3-fluorine thiodol each can meet the limit detection requirements of each isomer impurity impurities in fluorine thiodol.

Embodiment 3

[0059] Linear investigation:

[0060] Squeezing the impurity reserve solution, adding the dilution, diluted with grade grade, each impurities concentration is 0.05 μg / ml, 1 μg / ml, 2.5 μg / ml, 5 μg / ml, 7.5 μg / mL, 10 μg / ml. The solution was formulated as a linear solution according to the "Preparation of Toll Solution". Take 20 μl of the above linear solution, inject the liquid chromatograph, record the chromatogram, with the concentration of the horizontal coordinate, the peak area as ordinate, perform linear regression analysis, linearity, the correlation coefficient is 1.0000, the specific results see Figure 4 .

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Abstract

The invention relates to the technical field of chemical pharmacy, and particularly relates to a method for measuring isomer impurities in p-fluorothiophenol through an HPLC method. The method is used for carrying out quantitative detection on an isomer A, an isomer B and thiophenol in p-fluorothiophenol, wherein the isomer A is 2-fluorothiophenol, and the isomer B is 3-fluorothiophenol; and adding a TCEP solution into a p-fluorothiophenol sample, diluting to obtain a test solution, and detecting the test solution by high performance liquid chromatography to obtain the content of three impurities in the p-fluorothiophenol sample. According to the method, p-fluorothiophenol and related substances thereof can be effectively separated, generation of disulfide is prevented by adding the TCEP solution before testing, p-fluorothiophenol and impurities can exist in a single molecular state, and therefore the quantitative detection method is provided and is easy and convenient to operate, high in specificity, high in sensitivity and high in accuracy; and the quality of the p-fluorothiophenol is ensured to be controllable.

Description

Technical field [0001] The present invention relates to the field of chemical pharmaceutical techniques, and more particularly to a method of determining the amphiberic impurities of fluorine phenol in fluorinephenol in an HPLC method. Background technique [0002] The fluorine thirabus is an important medicine, pesticide and polymer intermediate, and can also be used for the detection of chemiluminescent agents, preparing nonlinear optical materials, and the like. The isomer impurity is introduced during the production of fluorophenols, and is unstable to fluorine phenol and its isomer impurity, and disulfide compounds are easily mutually mutually mutually. [0003] At present, there is no report to the detection method of fluorophenol neutral impurities, therefore, it is necessary to develop an HPLC method that effectively detects amphibular impurities of fluorine phenol. Inventive content [0004] It is an object of the present invention to overcome the above problems present...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/04
CPCG01N30/02G01N30/04G01N2030/047
Inventor 白玮丽杨玉娜刘洪明许多温乐
Owner 连云港杰瑞药业有限公司
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