Separation and purification method for acetylcysteine enantiomer

A technology of acetylcysteine ​​and enantiomers, which is applied in the field of separation and purification of acetylcysteine ​​enantiomers, can solve problems such as poor reproducibility, inaccurate quantification, and complicated separation and purification methods. Achieve accurate separation and simple operation

Active Publication Date: 2020-01-03
WUHAN GRAND HOYO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to overcome the defects in the prior art that the separation and purification method of N-acetylcysteine ​​enantiomers is complicated, and the deg

Method used

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  • Separation and purification method for acetylcysteine enantiomer
  • Separation and purification method for acetylcysteine enantiomer
  • Separation and purification method for acetylcysteine enantiomer

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0062] Example 1

[0063] 1. Apparatus and conditions:

[0064] High performance liquid chromatograph: Hitachi L2420;

[0065] Chromatographic column: cellulose coated chiral chromatographic column (model: Cellu-DR, 5μm, 4.6*250mm), the packing silica gel of this type of chromatographic column is coated with: cellulose-tris(3,5) dimethyl phenyl carbamate;

[0066] Mobile phase: n-hexane-isopropanol containing 0.5% acetic acid=80:20, the percentage is the volume percentage in isopropanol;

[0067] Flow rate: 1ml / min;

[0068] Column temperature: 25℃;

[0069] Injection volume: 20μL;

[0070] Detection wavelength: 220nm.

[0071] 2. Experimental methods and results:

[0072] (1) The preparation of the reference solution includes: accurately weigh the standard N-acetyl-L-cysteine ​​and N-acetyl-D-cysteine, and prepare them with diluent (chromatographic grade absolute ethanol) The concentration is a reference solution containing 0.1, 0.2, 0.5, 1.0 mg N-acetyl-L-cysteine ​​and 0.1, 0.2, 0.5, 1....

Example Embodiment

[0081] Example 2

[0082] Preparation of test solution 1: accurately weigh the standard N-acetyl-L-cysteine ​​and N-acetyl-D-cysteine, and use the diluent (chromatographic grade absolute ethanol) to prepare the concentration to each 1ml contains 0.5mg N-acetyl-L-cysteine ​​and 0.5mg N-acetyl-D-cysteine ​​mixed solution, as the test solution 1.

[0083] Take the test solution 1 and test it according to the conditions in Example 1. Repeat the injection for 5 times. The peak area is shown in Table 2.

[0084] Table 2 Test product 1 five injection repeatability

[0085]

[0086]

[0087] Note: " / " means not detected or not calculated.

[0088] It can be seen from Table 2 that the detection method in this application has good repeatability.

[0089] figure 1 This is the chromatogram of the solvent absolute ethanol in this example, Figure 2~6 It is the chromatogram of the first to fifth injections of the test solution 1.

[0090] by figure 2 It can be seen that the retention time of N-acetyl...

Example Embodiment

[0092] Example 3

[0093] Preparation of test solution 2: accurately weigh N-acetyl-DL-cysteine ​​(synthesized from DL cysteine ​​hydrochloride, and test the specific rotation as 0 according to AJI92 standard), and use diluent (chromatographic Grade absolute ethanol) as the test solution 2.

[0094] Take test solution 2 and test it according to the instrument and conditions in Example 1, and record the chromatogram. Such as Figure 7 Shown.

[0095] by Figure 7 Known:

[0096] (1) The retention time of N-acetyl-L-cysteine ​​is 14.28 min, the peak area is 617334, the height is 35513, and the area% is 47.568%; the retention time of N-acetyl-D-cysteine ​​is 15.21 min, peak area is 666171, height is 35225, area% is 51.331%; impurity peak retention time is 13.41min, peak area is 14298, height is 1100, area% is 1.102%; N-acetyl-L-cysteamine The resolution of acid and N-acetyl-D-cysteine ​​is greater than 1.5, the peak shape is good, no tailing, no protruding;

[0097] (2) Under the condi...

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Abstract

The invention discloses a separation and purification method for an acetylcysteine enantiomer. The separation and purification method is characterized in that an N-acetylcysteine enantiomer is separated by adopting high performance liquid chromatography; a mobile phase in the high performance liquid chromatography is an alkane solvent-isopropanol, and a volume ratio of the alkane solvent to the isopropanol is (70-83):(17-30); and the filler of a chromatographic column in the high performance liquid chromatography is a filler coated with a cellulose derivative represented by formula I. The separation and purification method can effectively separate the N-acetyl-L-cysteine and its enantiomer, further realizes the qualitative and quantitative analysis of the N-acetyl-L-cysteine and its enantiomer, and is of guiding significance for drug production and quality improvement.

Description

technical field [0001] The invention relates to the field of drug analysis and detection, in particular to a method for separating and purifying acetylcysteine ​​enantiomers. Background technique [0002] N-acetyl-L-cysteine ​​(Acetylcysteine, Ac-Cys), molecular formula: C 5 h 9 NO 3 S, molecular weight: 163.19. This product is white crystalline powder; has a garlic-like odor, sour taste; has hygroscopicity. Soluble in water, soluble in ethanol, insoluble in dichloromethane and ether; its structural formula is shown below. [0003] [0004] N-acetyl-L-cysteine ​​is a mucus-dissolving agent, which is suitable for dyspnea caused by a large amount of mucus obstruction, and dyspnea, and can also be used for postoperative dyspnea, acute and chronic bronchitis, and bronchiectasis , Pneumonia, tuberculosis, emphysema, etc. cause thick sputum and difficulty in expectoration, and are now mostly used for the treatment of idiopathic interstitial lung. In recent years, studies ...

Claims

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Application Information

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IPC IPC(8): C07C319/28C07C323/59G01N30/06B01D15/10B01D15/38
CPCB01D15/10B01D15/3833C07B2200/07C07C319/28G01N30/06C07C323/59
Inventor 李敬黄蕾杨磊梅雪臣何韺刘珍吕凡林
Owner WUHAN GRAND HOYO
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