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

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

Example Embodiment

[0038] Effect of diluent and split injection volume: Example 1

[0039] Acetonitrile concentration was taken as the reference sample diluent solution 206.4μg / mL of a (solution B), injection volume is 10 L, particularly poor prulifloxacin two diastereomer peaks, resolution and number of theoretical plates They are not satisfied, and there is a large solvent peak. Acetonitrile concentration was taken as the diluent 1032.1μg / mL of reference stock solution (solution a) and as the mobile phase at a concentration of diluent 200.2μg / mL solution of the two reference samples (solution d), respectively, sample and 10μL 2μL two ways injection prulifloxacin separation between the two pairs of enantiomers peaks of about 3.61 and 3.78, prulifloxacin peak almost no difference, but when the diluent is acetonitrile large solvent peak chromatogram see figure 1 .

[0040] Visible, while reducing acetonitrile diluted reference sample solution to the [mu] L injection volume, prulifloxacin enanti...

Example Embodiment

[0041] Effects on stability diluent: Example 2

[0042]A substantial solution (solution A) having a reaction product (solution A) having a acetonitrile concentration of 1032.1 [mu] g / ml after being placed for a period of time, respectively. (Solution D), according to the "experimental reagent and detection method 3 chromatographic conditions" injective analysis, wherein the solution A injection volume is 2 μl, and the solution D injection volume is 10 μl, and the stability of the solution is investigated.

[0043] RESULTS: Two enantiomeric peaks decreased by about 2% after 3 hours of use of mobile phase dilution, while the use of acetonitrile dilution is placed in Pullingazakian peak enantiomeric peak area decreased <0.2%, almost no Variety.

[0044] It can be seen that the use of acetonitrile is more stable to Pulby, and the use of mobile phase-diluted Pulley shadosaults is relatively unstable, and new match is required to be stored in 4 ° C.

Example Embodiment

[0045] Example 3: Effect of Chiral Flow Phase Additives on Split

[0046] Splitting the Pulling Sands enantiomers were split by L-phenylalanine, L-isoleucine and L-proline as a chiral ligand, wherein the concentration was about 1032.1 μg / ml. Pulley Sandy Reservoir (Solution A), and 2 μl of the injection amount.

[0047] RESULTS: Just only 1 color peak of Pluculi, Tuli Shaoxia, which cannot be split by L-phenylalanine and L-isoleucine when using L-phenylalanine and L-isoleucine. Pulley Shaxing has 2 color peaks that can achieve splitting of Pulling Saxi enantiomers. L-phenylalanine demolition Pulley sedae retention time is longer, increasing methanol ratio to 36% to investigate the separation of two enantiomeric peaks when the Pulling Sands enantiomer retention time is approximately The results are shown in Table 1.

[0048] Table 1 Effect of different chiral amino acids on retention time and separation

[0049]

[0050] As can be seen from the results of Table 1, although the ...

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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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