Flurbiprofen axetil enantiomer and liquid chromatography separation detection method of impurity a

A technology for flurbiprofen axetil and enantiomer, which is applied in the field of liquid chromatography separation and detection of flurbiprofen axetil enantiomer and impurity A, can solve the problem that separation results are not described in detail and chromatographic methods are complex and other problems, to achieve the effects of good reproducibility and stability, simple and easy chromatographic separation, and stable separation results

Active Publication Date: 2022-03-22
纳谱分析技术(苏州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chromatographic method of this invention is relatively complicated, and only quantitatively reports the baseline separation of the two pairs of enantiomers of flurbiprofen axetil, while the separation between the two pairs of enantiomers of the related substance impurity A And the separation results between them and the two pairs of enantiomers of flurbiprofen axetil are not described in detail

Method used

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  • Flurbiprofen axetil enantiomer and liquid chromatography separation detection method of impurity a
  • Flurbiprofen axetil enantiomer and liquid chromatography separation detection method of impurity a
  • Flurbiprofen axetil enantiomer and liquid chromatography separation detection method of impurity a

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Embodiment 1

[0045] Embodiment 1 uses the inventive method to separate and detect flurbiprofen axetil and its impurity A

[0046]1) Flurbiprofen axetil stock solution is diluted, as need testing solution; Get impurity A material dilution, as impurity A contrast solution; Get described need test solution and impurity A contrast solution mixing, as system suitability solution ;

[0047] 2) Two chromatographic columns using octadecylsilane bonded silica gel as filler and pentafluorophenylsilane bonded silica gel as filler;

[0048] 3) Using methanol and phosphoric acid aqueous solution as mobile phase, elution mode: isocratic elution.

[0049] Chromatographic conditions:

[0050] Chromatographic column: ChromCore C18 5μm (4.6×100mm) and ChromCore PFP 5μm (4.6×50mm) used in series

[0051] Mobile phase: 60 / 40 methanol / 0.1% phosphoric acid in water v / v

[0052] Column temperature: 30°C

[0053] Flow rate: 1mL / min

[0054] Injection volume: 5μL

[0055] Detection wavelength: 254nm

[005...

Embodiment 2

[0061] Embodiment 2 adopts the same chromatographic column and mobile phase of Embodiment 1, only the column temperature is different, and the enantiomers of flurbiprofen axetil and the corresponding isomers of impurity A are separated and detected at 20°C and 40°C respectively .

[0062] Chromatographic conditions:

[0063] Chromatographic column: ChromCore C18 5μm (4.6×100mm) and ChromCore PFP 5μm (4.6×50mm) used in series

[0064] Mobile phase: 60 / 40 methanol / 0.1% phosphoric acid in water v / v

[0065] Column temperature: 20°C / 40°C

[0066] Flow rate: 1mL / min

[0067] Injection volume: 5μL

[0068] Detection wavelength: 254nm

[0069] The preparation of need testing solution: get flurbiprofen axetil stock solution 10 μ L, add methanol 20mL dilution, as need testing solution; Get impurity A material solution 10 μ L, add methanol 20mL dilution, as impurity A contrast solution; Take need testing solution 1mL and impurity A control solution 10μL, mix well, as the system su...

Embodiment 3

[0072] Embodiment 3 adopts the same chromatographic column of embodiment 1, column temperature, mobile phase, only change the ratio of mobile phase methanol / phosphoric acid aqueous solution, separate and detect the enantiomer of flurbiprofen axetil and the corresponding isomer of impurity A

[0073] Chromatographic conditions:

[0074] Chromatographic column: ChromCore C18 5μm (4.6×100mm) and ChromCore PFP 5μm (4.6×50mm) used in series

[0075] Mobile phase: 65 / 35 methanol / 0.1% phosphoric acid in water v / v

[0076] Column temperature: 30°C

[0077] Flow rate: 1mL / min

[0078] Injection volume: 5μL

[0079] Detection wavelength: 254nm

[0080] The preparation of need testing solution: get flurbiprofen axetil stock solution 10 μ L, add methanol 20mL dilution, as need testing solution; Get impurity A material solution 10 μ L, add methanol 20mL dilution, as impurity A contrast solution; Take need testing solution 1mL and impurity A control solution 10μL, mix well, as the syst...

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Abstract

The invention provides a liquid chromatography separation and detection method for flurbiprofen axetil enantiomers and impurity A, wherein the flurbiprofen axetil material solution to be tested and the impurity A control solution are diluted and dissolved; The flurbiprofen axetil test solution is loaded onto an octadecylsilane-bonded silica gel column and a pentafluorophenylsilane-bonded silica gel series column, and the flurbiprofen axetil is separated and detected; methanol and phosphoric acid The aqueous solution is the mobile phase, and isocratic elution is carried out; after the elution is completed, use an ultraviolet detector to detect the signal intensity of the sample to be tested, and substitute the obtained signal intensity into the corresponding standard curve to calculate the flurbiprofen in the sample to be tested The concentration of the four components of ester and its enantiomer, impurity A and its enantiomer. The present invention can well separate the enantiomer of flurbiprofen axetil and the enantiomer of impurity A, with good separation degree, stable separation result, good method reproducibility and stability.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a liquid chromatography separation and detection method for flurbiprofen axetil enantiomers and impurity A. Background technique [0002] Flurbiprofen is a non-steroidal anti-inflammatory drug with anti-inflammatory and analgesic effects. Flurbiprofen axetil is the prodrug of flurbiprofen, and its chemical name is (±)-2-(2-fluoro-4-biphenyl)propionate-1-acetoxyethyl ester. It is widely used clinically, and can be used for analgesia after surgery and various cancers. The mechanism of action is mainly to inhibit the activity of arachidonic acid epoxidase, thereby inhibiting the synthesis of prostaglandins in pain and inflammatory responses. [0003] Flurbiprofen axetil has two pairs of enantiomers. The current clinically used flurbiprofen axetil is its racemate. The preparation type is fat emulsion injection. This dosage form is developed based on the concept of drug...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60G01N30/34
CPCG01N30/6039G01N30/34G01N2030/047
Inventor 杨洋刘晓东
Owner 纳谱分析技术(苏州)有限公司
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