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A method for the separation and detection of moxifloxacin hydrochloride intermediate and its enantiomers

A technology for moxifloxacin hydrochloride and enantiomers, which is applied in the field of separation and detection of moxifloxacin hydrochloride intermediates and enantiomers, can solve problems such as low content, achieve strong specificity and improve safety , Monitoring the effect of quality

Active Publication Date: 2016-06-08
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, because moxifloxacin hydrochloride intermediate I and its enantiomer II are enantiomers of each other, and the content of enantiomer II in the product of intermediate I is also relatively low, there is no related report can solve the above problems

Method used

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  • A method for the separation and detection of moxifloxacin hydrochloride intermediate and its enantiomers
  • A method for the separation and detection of moxifloxacin hydrochloride intermediate and its enantiomers
  • A method for the separation and detection of moxifloxacin hydrochloride intermediate and its enantiomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1 Detection of Moxifloxacin Hydrochloride Intermediate I and Enantiomer II

[0044] Detection conditions (reversed phase high performance liquid chromatography - chiral additive mobile phase):

[0045] Chromatographic column: Shim-packVP-ODSC18 (150mm×6.0mm, 5μm);

[0046] Chiral additive mobile phase: L-isoleucine copper sulfate solution (take 0.5g of copper sulfate pentahydrate and 0.5g of L-isoleucine, dissolve in 1000mL water, adjust the pH value to 4.5)-methanol (75:25) ;

[0047] Flow rate: 1.0mL / min;

[0048] Detection wavelength: 295nm;

[0049] Column temperature: 40°C;

[0050] Injection volume: 20 μL.

[0051] Detection steps:

[0052] Take an appropriate amount of moxifloxacin hydrochloride intermediate Ⅰ, dissolve it with mobile phase, and prepare a test solution containing about 0.2 mg per 1 mL; take an appropriate amount of enantiomer II reference substance, dissolve it with mobile phase, and prepare a solution of about Containing 0.2 mg of...

Embodiment 2

[0054] Example 2 Detection of Moxifloxacin Hydrochloride Intermediate I and Enantiomer II

[0055] Detection conditions (reversed phase high performance liquid chromatography - chiral additive mobile phase):

[0056] Chromatographic column: Shim-packVP-ODSC18 (150mm×6.0mm, 5μm);

[0057] Chiral additive mobile phase: L-isoleucine copper sulfate solution (take 0.5g of copper sulfate pentahydrate and 1.0g of L-isoleucine, dissolve in 1000mL water, adjust the pH value to 3.5)-methanol (75:25) ;

[0058] Flow rate: 1.0mL / min;

[0059] Detection wavelength: 295nm;

[0060] Column temperature: 40°C;

[0061] Injection volume: 20 μL.

[0062] Detection steps:

[0063] Take an appropriate amount of enantiomer II, dissolve it in mobile phase, and prepare a reference solution containing about 0.1 mg per 1 mL; take another appropriate amount of moxifloxacin hydrochloride intermediate I and enantiomer II, and dissolve it in mobile phase Prepare a system suitability solution contain...

Embodiment 3

[0065] Example 3 Detection of Moxifloxacin Hydrochloride Intermediate I and Enantiomer II

[0066] Detection conditions (normal phase high performance liquid chromatography - chiral column):

[0067] Chiral chromatography column: OD-H chiral column (DAICELCHIRALPAK, 250mm×4.6mm, 5μm);

[0068] Mobile phase: n-hexane-isopropanol (85:15);

[0069] Flow rate: 1.0mL / min;

[0070] Detection wavelength: 295nm;

[0071] Column temperature: 35°C;

[0072] Solvent: n-hexane-ethanol (20:80);

[0073] Injection volume: 20 μL.

[0074] Detection steps:

[0075] Take an appropriate amount of moxifloxacin hydrochloride intermediate Ⅰ, dissolve it with a solvent, and prepare a test solution containing about 0.5 mg per 1 mL; take an appropriate amount of enantiomer II, dissolve it with a solvent, and prepare a solution containing about 0.1 mg per 1 mL. Reference substance solution: Take the appropriate amount of the test solution and the reference substance solution, mix them in equal ...

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Abstract

The invention provides a separation and detection method for a moxifloxacin hydrochloride intermediate I and an enantiomer II thereof. The method is normal phase high-performance liquid chromatography, wherein the detection wavelength is 290-300 nm; a chiral chromatographic column uses cellulose-tris(3,5-dimethylphenylcarbamate) as a packing; n-hexane isopropanol is used as a mobile phase; the volume fraction of n-hexane is 80-90%. The method disclosed by the invention is high in specificity, simple, convenient, quick, accurate and reliable in determination result, so that the mass of moxifloxacin hydrochloride can be monitored effectively, and the drug safety can be improved.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a method for separating and detecting moxifloxacin hydrochloride intermediates and enantiomers thereof. Background technique [0002] Moxifloxacin hydrochloride is an 8-methoxyfluoroquinolone antibacterial drug, suitable for adults with upper and lower respiratory tract infections. Moxifloxacin hydrochloride was developed by Bayer AG of Germany. It was first listed in Germany in September 1999, in the United States in December of the same year, and officially launched in my country in 2002. Moxifloxacin has broad-spectrum antibacterial activity against Gram-positive bacteria, Gram-negative bacteria, anaerobic bacteria, acid-fast bacteria, and atypical microorganisms such as Mycoplasma, Chlamydia, and Legionella. [0003] Moxifloxacin hydrochloride can be synthesized by the following route: [0004] [0005] Among them, the moxifloxacin hydrochloride intermediate (4aS...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 孙毅夏玉立
Owner CHENGDU BAIYU PHARMA CO LTD
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