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Separation and measurement method of besifloxacin hydrochloride and isomer of besifloxacin hydrochloride

A technology for besifloxacin hydrochloride and enantiomers, applied in the field of analytical chemistry, can solve the problems of complex pretreatment process, failure to find, poor operability, etc., and achieve simple sample pretreatment process, accurate separation and detection , the effect of strong operability

Active Publication Date: 2015-03-25
SUNSHINE LAKE PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Zhangting WANG et al. screened a large number of chiral chromatographic columns and investigated possible chiral separation techniques in CHIRALITY 24:526–531 (2012), but failed to find a direct separation of besifloxacin hydrochloride and its enantiomer. Constructed method; Chinese patent application CN201110326752.3 adopts derivatization of besifloxacin hydrochloride, and then quantitatively detects it with a chiral chromatographic column (RP-HPLC) method, but the method is not operable and requires complex pre-processing The processing process also requires a complex derivatization process, and the analysis of enantiomers takes a long time for the entire analysis

Method used

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  • Separation and measurement method of besifloxacin hydrochloride and isomer of besifloxacin hydrochloride
  • Separation and measurement method of besifloxacin hydrochloride and isomer of besifloxacin hydrochloride
  • Separation and measurement method of besifloxacin hydrochloride and isomer of besifloxacin hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Instruments and Conditions

[0029] American Agilent 1260 high performance liquid chromatography system and workstation; automatic sampling;

[0030]

[0031]

Embodiment 2

[0033] Experimental procedure

[0034] Diluent or blank solution is mobile phase A phase / B phase=55 / 45(V:V);

[0035] Take about 20 mg of besifloxacin hydrochloride bulk drug (prepared according to the method disclosed in Chinese patent CN 200880003118), accurately weigh it into a 10 mL brown measuring bottle, dissolve it with a diluent and dilute to the mark, shake well, and use it as the test solution.

[0036] Get blank solution and need testing solution respectively, carry out high performance liquid chromatography analysis by the condition of embodiment 1, record chromatogram, the results are shown in figure 1 , figure 2 . figure 2 It shows that the separation and detection method of the present invention can separate besifloxacin hydrochloride and its enantiomers, and the high performance liquid chromatography shows that the separation degree is 3.56.

Embodiment 3

[0038] Take besifloxacin hydrochloride crude drug (prepared according to the method of CN 201310479217.0) about 20 mg of the test sample, accurately weigh it into a 10 mL brown volumetric flask, dissolve it ultrasonically with a diluent and dilute to the mark, shake well, and use it as the test sample solution.

[0039] Get need testing solution, carry out high performance liquid chromatography analysis according to the condition of example 1, record chromatogram, the results are shown in image 3 .

[0040] image 3 It is proved that this method can be used for the quality monitoring of besifloxacin hydrochloride, and the high performance liquid chromatography shows that the resolution is 3.74.

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Abstract

The invention relates to a separation and measurement method of besifloxacin hydrochloride and an isomer of besifloxacin hydrochloride. The method is characterized by adopting a chiral chromatographic column which takes cyclodextrin as a filler and adopting a mobile phase system formed by a buffer salt solution and an organic solvent. After the method is adopted, the besifloxacin and the enantiomer of the besifloxacin are effectively separated from each other, and the separation degree of the besifloxacin and the enantiomer of the besifloxacin reaches up to more than 3.5, so that the quality of besifloxacin hydrochloride can be accurately and effectively controlled. Compared with the existing patents and literatures, the method does not need a complicated derivative process and an expensive derivatization reagent on the whole, and is simple in sample pretreatment process, short in analysis time and high in operability. After the method is used, the besifloxacin and the optical isomer of the besifloxacin are simply, rapidly and accurately separated and detected.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and measuring besifloxacin hydrochloride and its optical isomers by liquid chromatography. Background technique [0002] The chemical name of besifloxacin hydrochloride is (R)-7-(3-aminohexahydro-1H-aza -1-base)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-carboxylic acid quinoline hydrochloride, its structure is as shown in formula (I) It is a new generation of fluoroquinolones for the treatment of bacterial conjunctivitis, which has shown superior bactericidal effect in clinical practice. The structural formula of besifloxacin hydrochloride is as shown in (I): [0003] [0004] In the structure of besifloxacin hydrochloride, a seven-membered ring side chain with a chiral center is connected to the 7-position, and the configuration of the chiral center is R-type, so there is a configuration of besifloxacin hydrochloride that is S-type The...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 陈超卢凌春饶万兵郭伟康刘国柱陈磊
Owner SUNSHINE LAKE PHARM CO LTD
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