A kind of detection method of 2,4-dimethylthiophenol related substances

A technology of dimethyl thiophenol and a detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve problems such as unsatisfactory separation effect, and achieve the effect of simple and convenient method, good repeatability and good specificity.

Active Publication Date: 2021-02-26
四川弘远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Considering that the molecular weight of 2,4-dimethylthiophenol is small and has certain volatility, the inventors of the present application also tried to adopt gas chromatography, using OP-WAX and DB-FFAP as chromatographic columns to pair 2,4 -Dimethylthiophenol-related substances were detected, but the separation effect was not satisfactory

Method used

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  • A kind of detection method of 2,4-dimethylthiophenol related substances
  • A kind of detection method of 2,4-dimethylthiophenol related substances
  • A kind of detection method of 2,4-dimethylthiophenol related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] 1. Drugs and reagents

[0083] With comparative example 1

[0084] 2. Main instruments

[0085] With comparative example 1

[0086] 3. Detection method

[0087] System suitability solution: Accurately weigh 10.30mg of 3-methylthiophenol, 11.40mg of 4-methylthiophenol, 10.01mg of 3,5-dimethylthiophenol, 3,4-dimethylthiophenol Phenol 10.09mg, 2,5-dimethylthiophenol 10.25mg, 2,4-dimethylthiophenol 10.16mg, 2,6-dimethylthiophenol 10.21mg were placed in the same 50ml measuring bottle, Dilute to the mark with methanol, accurately draw 2.5ml of the above solution, put it in a 50ml measuring bottle, and dilute to the mark with methanol.

[0088] Positioning solution: take 3-methylthiophenol, 4-methylthiophenol, 3,5-dimethylthiophenol, 3,4-dimethylthiophenol, 2,5-dimethylthiophenol Put appropriate amounts of thiophenol, 2,4-dimethylthiophenol, and 2,6-dimethylthiophenol into 25ml measuring bottles, and dilute with methanol to the mark.

[0089] Liquid chromatography detect...

Embodiment 2

[0095] This embodiment investigates the durability of the chromatographic method by changing the parameters of some chromatographic conditions, medicines and reagents and main instruments such as Comparative Example 1, and based on the following chromatographic conditions: using octadecylsilane bonded silica gel as a filler ( Kromasil, 100-5C18, 5μm, 250*4.6mm); use tetrabutylammonium hydroxide-containing phosphate buffer-methanol as the mobile phase; the flow rate is 1.0ml per minute; the detection wavelength is 230nm; the column temperature is 30°C.

[0096] This example examines the influence of chromatographic conditions such as the concentration of tetrabutylammonium hydroxide, the concentration of phosphate buffer, the type of phosphate, and the volume ratio of phosphate buffer to methanol on the detection system adaptability solution. Mainly investigate the effect of changing chromatographic conditions on the system adaptability of 2,4-dimethylthiophenol and 3-methylthio...

Embodiment 3

[0104] 1. Drugs and reagents

[0105] With comparative example 1

[0106] 2. Main instruments

[0107]With comparative example 1

[0108] 3. Detection method

[0109] Impurity control solution: Accurately weigh 11.62mg of 3-methylthiophenol, 14.40mg of 4-methylthiophenol, 13.74mg of 3,5-dimethylthiophenol, 2,5-dimethylthiophenol 12.98mg and 13.57mg of 2,6-dimethylthiophenol were placed in the same 50ml measuring bottle, diluted to the mark with methanol, and used as impurity control stock solution. Precisely draw 2.5ml of the above solution, put it in a 50ml measuring bottle, and dilute it to the mark with methanol to obtain the impurity control solution.

[0110] The test solution: Accurately weigh 0.1006g of 2,4-dimethylthiophenol, put it in a 50ml measuring bottle, dilute it to the mark with methanol, and use it as the test solution.

[0111] Liquid chromatography detection conditions: use octadecylsilane bonded silica gel as filler (Kromasil, 100-5C18, 5μm, 250*4.6mm)...

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Abstract

The invention provides a high-performance liquid chromatography detection method for related substances of 2,4-dimethylthiophenol. The liquid chromatography measurement conditions used are: the chromatographic column is filled with octadecylsilane bonded silica gel, and the mobile phase is phosphate buffer-methanol containing cation pairs. The method has the advantages of simple and convenient method, good specificity, high sensitivity, good repeatability, etc., and is suitable for the qualitative and quantitative detection of related substances in 2,4-dimethylthiophenol.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for separating and analyzing related substances of 2,4-dimethylthiophenol by high performance liquid chromatography. Background technique [0002] 2,4-dimethylbenzenethiol, also known as 2,4-dimethylbenzenethiol, is a commonly used pharmaceutical intermediate, and its structural formula is as follows: [0003] [0004] Molecular formula: C8H10S, molecular weight: 138.23. [0005] 2,4-Dimethylthiophenol is most commonly used in the synthesis of antidepressant drug Vortioxetine, according to the process route of 2,4-Dimethylthiophenol, the possible impurities are 3-methylthiophenol , 4-methylthiophenol, 2,5-dimethylthiophenol, 3,4-dimethylthiophenol, 3,5-dimethylthiophenol, 2,6-dimethylbenzene Thiophenol. The existence of these impurities will produce a series of side reactions, which will eventually greatly affect the purity of the product, and subsequent complicated processes ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 柯潇郑强张伟
Owner 四川弘远药业有限公司
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