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Separation and detection method of acetylcysteine enantiomer

A technology of acetylcysteine ​​and enantiomers, applied in the field of separation and detection of acetylcysteine, can solve the problems of unfavorable popularization, complex operation, low sensitivity, etc. Mild, short retention time effect

Active Publication Date: 2019-05-07
HUNAN WARRANT PHARM TECH DEV CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for separating and detecting acetylcysteine ​​enantiomers to solve the technical problems of complicated operation, low sensitivity and unfavorable popularization and use in the prior art

Method used

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  • Separation and detection method of acetylcysteine enantiomer
  • Separation and detection method of acetylcysteine enantiomer
  • Separation and detection method of acetylcysteine enantiomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Sample to be tested 1: Accurately measure 1ml of acetylcysteine ​​solution for inhalation, the pH of the solution is neutral, put it in a 100ml measuring bottle, dilute with methanol to the mark, shake well, take 5ml precisely, put it in a 10ml measuring bottle ,stand-by;

[0076] Take another 25 mg of acetylcysteine ​​enantiomer reference substance, accurately weigh it, put it in a 25ml measuring bottle, add 3ml of 0.05mol / L sodium hydroxide methanol solution, dilute to the mark with methanol, shake well, and use it as a reference substance Mother liquor: Accurately measure 1ml of the mother liquor of the reference substance, put it in a 20ml measuring bottle, dilute to the mark with methanol, shake well, accurately measure 1ml, add it to the above-mentioned sample solution to be used, and then precisely add the derivative reagent (R)-( +)-a-methylbenzyl isocyanate 10μl, plugged tightly, shake well, put in 55°C water bath for 20min, let cool, dilute to the mark with me...

Embodiment 2

[0081] Sample to be tested 1: Accurately measure 1ml of acetylcysteine ​​solution for inhalation. The pH of the solution is neutral. in a bottle, ready to use;

[0082] Take another 25 mg of acetylcysteine ​​isomer reference substance, accurately weigh it, put it in a 25 ml measuring bottle, add 3 ml of 0.05 mol / L sodium hydroxide isopropanol solution, dilute to the mark with isopropanol, shake well, and use as Reference substance mother liquor: accurately measure 1ml of the reference substance mother liquor, put it in a 20ml measuring bottle, dilute to the mark with isopropanol, shake up, accurately measure 1ml, add it to the above-mentioned sample solution to be used, and then precisely add the derivative reagent ( S)-(-)-a-methylbenzyl isocyanate 10μl, plugged tightly, shake well, put in 50°C water bath for 18min, let cool, dilute to the mark with isopropanol, shake well, as a mixed solution;

[0083] Accurately measure 10 μl each of the reference substance solution and th...

Embodiment 3

[0086] Sample to be tested 2: Accurately measure 1ml of acetylcysteine ​​solution for inhalation. The pH of the solution is neutral. in a bottle, ready to use;

[0087] Take another 25 mg of acetylcysteine ​​isomer reference substance, accurately weigh it, put it in a 25 ml measuring bottle, add 3 ml of 0.05 mol / L sodium hydroxide isopropanol solution, dilute to the mark with isopropanol, shake well, and use as Reference substance mother liquor: accurately measure 1ml of the reference substance mother liquor, put it in a 20ml measuring bottle, dilute to the mark with isopropanol, shake up, accurately measure 1ml, add it to the above-mentioned sample solution to be used, and then precisely add the derivative reagent ( S)-(-)-a-methylbenzyl isocyanate 10μl, plugged tightly, shake well, put in 50°C water bath for 18min, let cool, dilute to the mark with isopropanol, shake well, as a mixed solution;

[0088] Accurately measure 10 μl each of the reference substance solution and th...

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Abstract

The invention discloses a separation and detection method of an acetylcysteine enantiomer. The method comprises the following steps: performing derivatization reaction in an organic solvent by using aderivatization reagent, N-acetyl-L-cysteine and an enantiomer thereof, so as to prepare a derivative product of N-acetyl-L-cysteine and isomers thereof; and performing separation and detection by using normal phase high-performance liquid chromatography, wherein the derivatization reagent is isocyanate. According to the separation and detection method of the acetylcysteine enantiomer, the derivatization reagent, N-acetyl L-cysteine and the enantiomer thereof are reacted, so that the mutual attraction effect between the stationary phase in the chromatographic column and the chiral substance tobe separated is increased according to the chiral separation mechanism by adopting precolumn derivatization normal phase high-performance liquid chromatography, and the chiral separation selectivityis effectively improved. The method is simple and convenient to operate, short in consumption time and easy to popularize and use.

Description

technical field [0001] The invention relates to the field of separation and detection of acetylcysteine, in particular to a method for separation and detection of acetylcysteine ​​enantiomers. Background technique [0002] Acetylcysteine, chemical name N-acetyl-L-cysteine, molecular formula C 5 h 9 NO 3 S, is a respiratory mucus dissolving agent, which can decompose white mucus and thick sputum, so as to improve the patient's respiratory condition. Acetylcysteine ​​drugs have been approved for marketing at home and abroad, and are used to treat respiratory diseases with excessive thick mucous secretions, such as: acute bronchitis, chronic bronchitis and its deterioration, emphysema, and sticky substance obstruction syndrome and bronchiectasis. [0003] Acetylcysteine ​​contains a chiral center, and the chemical name of its enantiomer is N-acetyl-D-cysteine, which is an important indicator for the quality control of acetylcysteine. Patent 201010297844.9 discloses a metho...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 周志刚庞永清龙辉徐燕黄本东
Owner HUNAN WARRANT PHARM TECH DEV CO LTD
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