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Resolution method of prulifloxacin enantiomers

A technology of prulifloxacin and enantiomers, applied in material separation, material analysis, measuring devices, etc., can solve the problem of no split report and achieve good linear relationship and simple operation

Pending Publication Date: 2021-11-19
江西省药品检验检测研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to understand the ratio of left and right-handed prulifloxacin in the drug, it is necessary to establish a corresponding enantiomer resolution method, but there are almost no reports on the separation of the enantiomers of the drug at home and abroad

Method used

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  • Resolution method of prulifloxacin enantiomers
  • Resolution method of prulifloxacin enantiomers
  • Resolution method of prulifloxacin enantiomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Effect of Diluent and Injection Volume on Resolution

[0039] Take acetonitrile as the reference substance sample solution one (solution b) with a concentration of 206.4 μg / mL as the diluent. When the injection volume is 10 μL, the peak shapes of the two enantiomers of prulifloxacin are particularly poor. All unsatisfactory, and have bigger solvent peak. Take acetonitrile as the reference substance stock solution (solution a) with a diluent concentration of 1032.1 μg / mL and reference substance sample solution 2 (solution d) with a mobile phase as a diluent concentration of 200.2 μg / mL, and inject 2 μL and 10 μL respectively , the separation between the two enantiomer peaks of prulifloxacin injected by the two methods is about 3.61 and 3.78, and there is almost no difference in the peak shape of prulifloxacin, except that the solvent peak is larger when acetonitrile is used as the diluent, see the chromatogram figure 1 .

[0040] It can be seen that when the...

Embodiment 2

[0041] Example 2: Effect of Diluent on Stability

[0042]Respectively take the reference substance stock solution (solution a) with acetonitrile as the diluent concentration of 1032.1 μg / mL and the reference substance sample solution 2 with the mobile phase as the diluent concentration of 200.2 μg / mL just prepared and after standing for a period of time. (Solution d), according to "Experimental Reagents and Detection Method 3 Chromatographic Conditions", sample injection analysis, wherein, the injection volume of solution a is 2 μL, and the injection volume of solution d is 10 μL, and the stability of the solution is investigated.

[0043] Results: When diluting with mobile phase, the peak area of ​​the two enantiomers of prulifloxacin decreased by about 2% after being placed for 3 hours, and the peak area of ​​the enantiomer of prulifloxacin peak decreased by <0.2% when diluted with acetonitrile for 80 h, almost no Variety.

[0044] It can be seen that the stability of pruli...

Embodiment 3

[0045] Example 3: Effect of Chiral Mobile Phase Additives on Resolution

[0046] The enantiomers of prulifloxacin were separated and analyzed by using L-phenylalanine, L-isoleucine and L-proline as chiral ligands, among which, the selected concentration was about 1032.1 μg / mL For the prulifloxacin reference stock solution (solution a), the injection volume was 2 μL for the experiment.

[0047] Results: When L-proline was used, prulifloxacin had only one chromatographic peak, and the enantiomers of prulifloxacin could not be resolved; while L-phenylalanine and L-isoleucine were used in the chromatogram Prulifloxacin has 2 chromatographic peaks, which can realize the separation of prulifloxacin enantiomers. The retention time of the enantiomer of prulifloxacin is longer when L-phenylalanine is resolved, and the proportion of methanol is increased to 36% to investigate the separation between the two enantiomer peaks when the retention time of the enantiomer of prulifloxacin is s...

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Abstract

The invention belongs to the technical field of pharmacy, and particularly relates to a resolution method of prulifloxacin enantiomers. According to the resolution method, a chiral coordination exchange mobile phase additive HLPC method is adopted, a chiral additive is added into a mobile phase and is coordinated with the prulifloxacin enantiomer to form a ternary complex of two diastereomers, and then resolution of the enantiomers is carried out on a chromatographic column of an achiral stationary phase. The method comprises the following specific steps: (1), performing preparation of a sample solution; and (2), performing separation steps and conditions. The method for resolution of the prulifloxacin enantiomer by using the chiral coordination exchange mobile phase additive HLPC method is successfully established, and the method is simple to operate, economical and practical, has good linear relation, precision and sensitivity, and can be used for resolution and quality control of the prulifloxacin enantiomer.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a method for splitting prulifloxacin enantiomers. Background technique [0002] The chirality of drug molecules is closely related to the pharmacological activity, toxicity and pharmacokinetic properties of drugs. When the enantiomers of chiral drugs enter the organism, they will be recognized and matched as different molecules. Therefore, enantiomers have stereoselectivity in pharmacodynamics, pharmacokinetics and toxicology, resulting in their biological activity, metabolic process and Significant differences may exist in terms of toxicity, the most typical example being the "reactin" incident in the 1960s. In view of the great difference in the pharmacological activity and toxicity of enantiomers of chiral compounds, it is very necessary and important to carry out studies on enantiomer chemistry (purity identification, inspection, etc.), pharmacology, toxicology,...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02Y02P20/55
Inventor 陈希鄢雷娜张文婷周敏肖小武段和祥陈伟康任琦
Owner 江西省药品检验检测研究院
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