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High performance liquid chromatography method for analysis of alkyl chloride compound

A high-performance liquid chromatography and alkyl acid chloride technology, which is applied in the field of high-performance liquid chromatography to analyze alkyl acid chloride compounds, can solve problems such as inability to separate R and S configurations, strong pungent odor, and needs to be improved. Sensitivity, convenient liquid phase detection, good elution and separation effect

Inactive Publication Date: 2016-02-03
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the fact that alkyl acid chlorides are generally colorless transparent fuming liquids with a strong pungent odor, they are easily decomposed when encountering water and alcohol, are easy to deteriorate, and have no ultraviolet absorption
Ordinary chromatography cannot separate the R and S configurations in such chiral products
[0007] Therefore, the current method for the analysis of alkyl acid chlorides still needs to be improved

Method used

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  • High performance liquid chromatography method for analysis of alkyl chloride compound
  • High performance liquid chromatography method for analysis of alkyl chloride compound
  • High performance liquid chromatography method for analysis of alkyl chloride compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 adopts high performance liquid chromatography to measure the content of S-acetoxy propionyl chloride enantiomer

[0042] Instrument: Agilent1100 HPLC, 1100 UV detector

[0043] Chromatographic column: CHIRALPAKAS-H (150×4.6mm, 5μm);

[0044] Mobile phase: n-hexane: isopropanol = 85: 15 (v / v)

[0045] Flow rate: 1.0mL / min

[0046] Detection wavelength: 210nm

[0047] Column temperature: 35°C

[0048] Injection volume: 2μL

[0049] Diluent: n-Hexane: Isopropanol = 50:50 (v / v)

[0050] Run time: 25 minutes

[0051] Experimental steps:

[0052] Derivatization method: Dissolve about 80 mg of benzylamine in dichloromethane, then slowly add about 60 mg of S-acetoxypropionyl chloride sample under ice bath, stir for 10 minutes after the addition, filter the solid, and wash with a small amount of dichloromethane , the collected solid is the derivatized sample of S-acetoxypropionyl chloride, and is set aside. (Note: The product obtained by derivatization of S-c...

Embodiment 2

[0086] Example 2 Determination of the content of S-acetoxybutyryl chloride enantiomers by high performance liquid chromatography

[0087] Instrument: Agilent1100 HPLC, 1100 UV detector

[0088] Chromatographic column: CHIRALPAKAS-H (150×4.6mm, 5μm);

[0089] Mobile phase: n-hexane: isopropanol = 85: 15 (v / v)

[0090] Flow rate: 1.0mL / min

[0091] Detection wavelength: 210nm

[0092] Column temperature: 35°C

[0093] Injection volume: 2μL

[0094] Diluent: n-Hexane: Isopropanol = 50:50 (v / v)

[0095] Run time: 25 minutes

[0096] Experimental steps:

[0097] Derivation step: Dissolve about 40 mg of benzylamine in dichloromethane, then slowly add about 32 mg of acid chloride under ice bath, stir for 10 minutes after the addition, filter the solid, wash with a small amount of dichloromethane, and collect the solid as acetoxy The derivatized sample of butyryl chloride is reserved.

[0098] Sample preparation: take about 20mg of the derivatized sample and place it in a 5ml...

Embodiment 3

[0100] Example 3 Determination of the content of S-acetoxypropionyl chloride enantiomers by high performance liquid chromatography

[0101] Instrument: Agilent1100 HPLC, 1100 UV detector

[0102] Chromatographic column: CHIRALPAKAD-H (250×4.6mm, 5μm);

[0103] Mobile phase A: n-hexane: ethanol = 90: 10 (v / v)

[0104] Flow rate: 1mL / min

[0105] Detection wavelength: 210nm

[0106] Column temperature: 35°C

[0107] Injection volume: 2μL

[0108] Diluent: n-Hexane: Ethanol = 50:50 (v / v)

[0109] Run time: 25 minutes

[0110] Derivatization step: Dissolve about 40 mg of benzylamine in dichloromethane, then slowly add about 30 mg of acid chloride under ice bath, stir for 10 minutes after the addition, filter the solid, wash with a small amount of dichloromethane, collect the solid as acetoxy The derivatized sample of propionyl chloride is used for later use.

[0111] Sample preparation: Take about 20mg of the derivatized sample in a 5ml volumetric flask, dissolve it with a...

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Abstract

The invention discloses a high performance liquid chromatography method for analysis of alkyl chloride compound. The analytical conditions are as below: chromatography column uses a polysaccharide coated chiral chromatographic column; a mixed solution containing a derivative reagent, a sample to be measured and a diluent is used as the solution to be measured; a first mixed solution containing a first organic solvent and a second organic solvent is used as a mobile phase; a mixed solution containing a first organic solvent and a second organic solvent is used as a diluent; and the first organic solvent is an organic hydrocarbon solvent, and the second organic solvent is an organic alcohol solvent. The method can fast and efficiently separate enantiomers of alkyl compounds, and effectively control of the quality of chiral acyl chloride compounds. The detection method has the advantages of high sensitivity, good repeatability, high accuracy, wide application range, low cost and convenient operation, and can effectively control the product quality.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular, the invention relates to a method for analyzing alkyl acid chloride compounds by high performance liquid chromatography. Background technique [0002] Alkyl acid chloride compounds (compounds shown in formula 1 and formula 2) are a class of important fine chemical intermediates, which have wide application value in chemical industry, medicine, materials and environment and life sciences, such as S-acetoxy Propionyl chloride, which is used in the synthesis of iopamidol, a widely used contrast agent in diagnostic investigations via X-rays. [0003] [0004] Among them, X 1 、X 2 Each independently is any one of the following groups: C 1 -C 3 alkyl. [0005] Alkyl acid chlorides can exert important physiological activities. In organic asymmetric synthesis, the ideal goal of technicians is to directly obtain a single and pure optical isomer, but the actual product often c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 林娟戚争春钱丽娜王一婷
Owner WATERSTONE PHARMA WUHAN
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