Method for detecting 1-bromo-4-chlorobutan in brexpiprazole intermediate

A technology of epipiprazole and detection method is applied in the detection field of 1-bromo-4-chlorobutane, and can solve the report of detection method of 1-bromo-4-chlorobutane, low HPLC detection signal response and accurate detection Difficulty and other problems, to achieve the effect of excellent linear relationship, high recovery rate and good stability

Active Publication Date: 2017-05-31
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, 1-bromo-4-chlorobutane has a small UV absorption and a low HPLC detection signal response, making accurate detection difficult.
There is no report on the detection method of 1-bromo-4-chlorobutane in ebiprazole intermediate

Method used

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  • Method for detecting 1-bromo-4-chlorobutan in brexpiprazole intermediate
  • Method for detecting 1-bromo-4-chlorobutan in brexpiprazole intermediate
  • Method for detecting 1-bromo-4-chlorobutan in brexpiprazole intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] 1. Determination of detection wavelength

[0051] Accurately weigh an appropriate amount of ebiprazole intermediate, and prepare a solution with a concentration of 20 μg / mL with methanol as the test solution.

[0052] Accurately weigh an appropriate amount of the reference substance (1-bromo-4-chlorobutane), and prepare a solution with a concentration of 20 μg / mL with methanol as the reference substance solution.

[0053] Take the above-mentioned test solution and reference solution, and scan in the wavelength range of 200nm to 400nm. The test results are shown in Table 1.

[0054] Table 1 UV scanning results of test solution and reference solution

[0055] project Peak wavelength(nm) the peak Valley wavelength(nm) valley Test solution 215.7 0.617 278 0.226 Reference solution 215.2 0.834 292 0.006

[0056] The test results show that the detection wavelength in the range of 210nm-220nm is suitable for the HPLC detection method of...

Embodiment 2

[0081] Chromatographic column filler: octadecylsilane-bonded silica gel is used as the filler;

[0082] The model of the chromatographic column is Waters Symmetry C18, and the specifications are: the inner diameter is 4.6 mm, the length is 250 mm, and the filler particle size is 5 μm;

[0083] Mobile phase: acetonitrile-0.02mol / L dipotassium hydrogen phosphate (adjust pH to 3.0 with phosphoric acid)=45:55;

[0084] Column temperature: 35°C;

[0085] Flow rate: 1.0mL / min;

[0086] Detection wavelength: 215nm;

[0087] Injection volume: 20 μL.

[0088] Carry out system suitability test according to the method for embodiment 1, the result shows: The degree of separation is 19.715, the number of theoretical plates (calculated by 1-bromo-4 chlorobutane chromatographic peak) is 5913, and the tailing factor of 1-bromo-4 chlorobutane chromatographic peak is 1.051.

[0089] It can be seen that the chromatographic conditions can accurately detect the content of 1-bromo-4 chlorobuta...

Embodiment 3

[0091] Chromatographic column filler: octadecylsilane-bonded silica gel is used as the filler;

[0092] The model of the chromatographic column is Waters Symmetry C18, and the specifications are: the inner diameter is 4.6 mm, the length is 250 mm, and the filler particle size is 5 μm;

[0093] Mobile phase: acetonitrile-0.02mol / L dipotassium hydrogen phosphate (adjust pH to 3.0 with phosphoric acid)=55:45;

[0094] Column temperature: 35°C;

[0095] Flow rate: 1.0mL / min;

[0096] Detection wavelength: 215nm;

[0097] Injection volume: 20 μL.

[0098] Carry out system suitability test according to the method for embodiment 1, the result shows: between ebiprazole intermediate (retention time is 3.7707min) and 1-bromo-4 chlorobutane reference substance (for its retention time is 9.666min) The degree of separation is 5.011, the number of theoretical plates (calculated by 1-bromo-4 chlorobutane chromatographic peak) is 19855, and the tailing factor of 1-bromo-4 chlorobutane chr...

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Abstract

The invention discloses a method for detecting 1-bromo-4-chlorobutan in a brexpiprazole intermediate. According to the method, by adopting a chromatographic column of octadecyl silane bonded silica gel, and the 1-bromo-4-chlorobutan in the brexpiprazole intermediate can be effectively separated and detected. A detection result is accurate and reliable, and the method has multiple advantages such as excellent linear relation, high precision, good stability, good repeatability, high recovery and simple and convenient operation, and is suitable for being popularized and applied.

Description

technical field [0001] The invention relates to a detection method of 1-bromo-4-chlorobutane in an ebiprazole intermediate, in particular to a detection method of 1-bromo-4-chlorobutane. Background technique [0002] Ebiprazole is an antipsychotic drug used to treat schizophrenia. The medicinal chemical, called Brexpiprazole, is also approved as an adjunctive treatment for major depressive disorder (MDD), a serious psychiatric disorder that causes persistent sadness, frustration or anger. Schizophrenia is a chronic, severe and disabling brain disorder that can cause delusions and hallucinations. According to the National Institute of Mental Health, the disorder affects about 1 percent of Americans. At its worst, MDD can lead to suicide, killing around 1 million people a year, according to the World Health Organization. The drug was launched in the U.S. market by Otsuka Pharmaceutical Company in August 2015, and is currently not listed in China. As an intermediate product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74
Inventor 宋务雄孙毅
Owner CHENGDU BAIYU PHARMA CO LTD
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