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HPLC analysis method of n-(phenylsulfonyl)benzamide compounds

An analytical method and technology of substances, applied in the direction of analytical materials, material separation, instruments, etc.

Active Publication Date: 2020-11-10
SHANGHAI YASHENG MEDICAL TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1) Only one enantiomer has the required pharmacological activity, while the other enantiomer has no pharmacological effect, for example: two enantiomers of the β-receptor blocker propranolol The in vitro activity of the non-steroidal anti-inflammatory drug naproxen (S)-configuration enantiomer is 35 times stronger than that of its enantiomer

Method used

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  • HPLC analysis method of n-(phenylsulfonyl)benzamide compounds
  • HPLC analysis method of n-(phenylsulfonyl)benzamide compounds
  • HPLC analysis method of n-(phenylsulfonyl)benzamide compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Embodiment 1: the mensuration of formula I compound chiral purity

[0100] High performance liquid chromatography conditions:

[0101] Chromatographic column: Daicel Chiralpak IC (250 mm×4.6 mm, 5.0 µm).

[0102] Mobile phase volume ratio: n-hexane / isopropanol / dichloromethane / tetrahydrofuran / acetic acid / diethylamine=700 / 70 / 80 / 150 / 1 / 0.2.

[0103] Detection wavelength: 282nm.

[0104] Flow rate: 2.0ml / min.

[0105] The column temperature was 33°C.

[0106] Injection volume: 20 μl.

[0107] Diluent: The volume ratio of dichloromethane to mobile phase is 1:1.

[0108] Experimental procedure

[0109] Solution preparation: Take about 20 mg of the compound of formula I, accurately weigh it and place it in a 10 ml measuring bottle, add 5 ml of dichloromethane, after the sample is completely dissolved, dilute to the mark with mobile phase, shake well, and use it as the test solution I;

[0110] Take 1 tablet of the compound of formula I and grind it into fine powder, tran...

Embodiment 2

[0119] Embodiment 2: the mensuration of formula I compound chiral purity

[0120] High performance liquid chromatography conditions:

[0121] Chromatographic column: Daicel Chiralpak IC (250 mm×4.6 mm, 5.0 µm).

[0122] Mobile phase volume ratio: diethylamine / triethylamine / tetrahydrofuran / ethanol / dichloromethane / n-hexane=1 / 1 / 120 / 130 / 50 / 700.

[0123] Detection wavelength: 287nm.

[0124] Flow rate: 1.0ml / min.

[0125] Column temperature: 33°C.

[0126] Injection volume: 20 μl.

[0127] Diluent: The composition is the same as that of the mobile phase.

[0128] Experimental procedure

[0129] Solution preparation: take about 20mg of the compound of formula I, accurately weigh it and place it in a 50ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0130] Take about 20mg of (S)-compound reference substance of formula I, accurately weigh it and place it in a 50ml measuring bottle, dissolve it with a diluent an...

Embodiment 3

[0136] Embodiment 3: the mensuration of formula I compound chiral purity

[0137] High performance liquid chromatography conditions:

[0138] Chromatographic column: Daicel Chiralpak IC (250 mm×4.6 mm, 5.0 µm).

[0139] Mobile phase volume ratio: tetrahydrofuran / ethanol / dichloromethane / n-hexane=150 / 100 / 50 / 700.

[0140] Detection wavelength: 282nm.

[0141] Flow rate: 1.0ml / min.

[0142] Column temperature: 33°C.

[0143] Injection volume: 10 μl.

[0144] Diluent: The volume ratio of dichloromethane to mobile phase is 1:1.

[0145] Experimental procedure

[0146] Solution preparation: Take about 30 mg of the compound of formula I, accurately weigh it and place it in a 20 ml measuring bottle, dissolve it with 10 ml of dichloromethane, dilute to the mark with mobile phase, shake well, and use it as the test solution;

[0147] Take about 30mg of (S)-compound reference substance of formula I, accurately weigh it and place it in a 20ml measuring bottle, dissolve it with 10ml of...

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Abstract

The invention discloses an HPLC analysis method for N-(phenylsulfonyl)benzamide compounds. The present invention relates to a kind of HPLC analytical method of substance X; Described substance X is the compound shown as formula I-A and / or I-B; Described HPLC analytical method comprises the following steps: in chiral chromatographic column, use The mobile phase substance X can be eluted; the chiral chromatographic column is a polysaccharide derivative solvent-resistant chiral chromatographic column; the column temperature of the chiral chromatographic column is 25-35 ° C; the elution Off is isocratic elution; described mobile phase comprises alkane solvent, alcohol solvent, halogenated hydrocarbon solvent and ether solvent, and by volume parts, described alkane solvent is 600-800 parts, so The alcohol solvent is 50-350 parts, the halogenated hydrocarbon solvent is 30-100 parts, and the ether solvent is 50-200 parts. The analysis method of the invention can separate the isomers and can accurately determine the purity of the isomers.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to an HPLC analysis method for N-(phenylsulfonyl)benzamide compounds. Background technique [0002] Apoptosis, the process of programmed cell death, is an essential biological process for tissue homeostasis. In mammals, it has been shown to regulate early embryonic development. Later in life, cell death is a default mechanism by which potentially dangerous cells, such as those carrying cancerous defects, are removed. Several apoptotic pathways are known. One of the most important apoptotic pathways involves the Bcl-2 family of proteins, which are key regulators of the mitochondrial (also called "intrinsic") pathway of apoptosis. See Danial and Korsmeyer, Cell 776:205-219 (2004). Structural homology domains BH1, BH2, BH3 and BH4 are characteristic of Bcl-2 family proteins. The Bcl-2 protein family can be further divided into three subfamilies, depending on how ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8696
Inventor 张现新倪友凤孙智鹏陈明圆张小妮
Owner SHANGHAI YASHENG MEDICAL TECH
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