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An HPLC method for detecting N-(4-(benzyloxy)benzylidene) aniline in N-(4-(benzyloxy)benzylidene)-4-fluoroaniline

A technology of benzyloxybenzylidene aniline and benzyloxybenzylidene, which is applied in the field of HPLC analysis of 4-benzyloxybenzylidene aniline, can solve the problem of poor separation between impurities and main peaks, poor durability, Difficult to detect and other problems, to achieve the effect of improving detection sensitivity and durability, improving detection sensitivity, and extending retention time

Active Publication Date: 2017-11-17
NANJING SIMCERE DONGYUAN PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There is no record in the prior art about the specific analytical method for detecting impurity 4-benzyloxybenzylidene aniline from 4-benzyloxybenzylidene-4-fluoroaniline, and select common C18 chromatographic column for use, impurity and The resolution of the main peak is poor. In short, the general detection method has poor resolution, low response, poor durability, and it is difficult to detect when the limit is small

Method used

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  • An HPLC method for detecting N-(4-(benzyloxy)benzylidene) aniline in N-(4-(benzyloxy)benzylidene)-4-fluoroaniline
  • An HPLC method for detecting N-(4-(benzyloxy)benzylidene) aniline in N-(4-(benzyloxy)benzylidene)-4-fluoroaniline
  • An HPLC method for detecting N-(4-(benzyloxy)benzylidene) aniline in N-(4-(benzyloxy)benzylidene)-4-fluoroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Chromatographic conditions:

[0030] Instrument: Agilent1260HPLC

[0031] Chromatographic column: Pentafluorophenyl column (4.6×100mm, 2.6μm)

[0032] Mobile phase A: Phosphate buffer (Weigh 1.36g of potassium dihydrogen phosphate, add 1000ml of water to dissolve, add 5ml of triethylamine, adjust pH to 6.8 with phosphoric acid)

[0033] Mobile Phase B: Acetonitrile: Methanol—1:1

[0034] Mobile phase: mobile phase A-mobile phase B (40:60)

[0035] Column temperature: 35°C

[0036] Flow rate: 1.0ml / min

[0037] Detection wavelength: 320nm

[0038] Injection volume: 5ul

[0039] Analysis time: record the chromatogram to twice the retention time of the main component peak

[0040] Solvent: Acetonitrile

[0041] 2) Sample preparation:

[0042] Take an appropriate amount of 4-benzyloxybenzylidene-4-fluoroaniline, add a solvent to prepare a solution containing 3.0 mg of 4-benzyloxybenzylidene-4-fluoroaniline per ml, as the test solution.

[0043] Take an appropri...

Embodiment 2

[0046] 1) Chromatographic conditions:

[0047] Instrument: Agilent1260HPLC

[0048] Chromatographic column: Pentafluorophenyl column (4.6×100mm, 2.6μm)

[0049] Mobile phase A: Phosphate buffer (Weigh 1.36g of potassium dihydrogen phosphate, add 1000ml of water to dissolve, add 5ml of triethylamine, adjust pH to 11.0 with phosphoric acid)

[0050] Mobile Phase B: Acetonitrile: Methanol—1:1

[0051] Mobile phase: mobile phase A-mobile phase B (40:60)

[0052] Column temperature: 35°C

[0053] Flow rate: 1.0ml / min

[0054] Detection wavelength: 320nm

[0055] Injection volume: 5ul

[0056] Analysis time: record the chromatogram to twice the retention time of the main component peak

[0057] Solvent: Acetonitrile

[0058] 2) Sample preparation:

[0059] Take an appropriate amount of 4-benzyloxybenzylidene-4-fluoroaniline, add a solvent to prepare a solution containing 3.0 mg of 4-benzyloxybenzylidene-4-fluoroaniline per ml, as the test solution.

[0060] Take an appropr...

Embodiment 3

[0063] 1) Chromatographic conditions:

[0064] Instrument: Agilent1260HPLC

[0065] Chromatographic column: Pentafluorophenyl column (4.6×100mm, 2.6μm)

[0066] Mobile phase A: water (add 5ml triethylamine to 1000ml water, adjust the pH to about 2.0 with phosphoric acid)

[0067] Mobile Phase B: Acetonitrile: Methanol—1:1

[0068] Mobile phase: mobile phase A-mobile phase B (20:80)

[0069] Column temperature: 30°C

[0070] Flow rate: 1.0ml / min

[0071] Detection wavelength: 320nm

[0072] Injection volume: 5ul

[0073] Analysis time: record the chromatogram to twice the retention time of the main component peak

[0074] Solvent: mobile phase B

[0075] 2) Sample preparation:

[0076] Take an appropriate amount of 4-benzyloxybenzylidene-4-fluoroaniline, add a solvent to prepare a solution containing 3.0 mg of 4-benzyloxybenzylidene-4-fluoroaniline per ml, as the test solution.

[0077] Take an appropriate amount of SCR-5014 reference substance, add solvent to make a ...

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Abstract

The invention discloses an HPLC method for detecting an impurity that is N-(4-(benzyloxy)benzylidene) aniline in N-(4-(benzyloxy)benzylidene)-4-fluoroaniline. In the method, a phenyl bonded silica gel chromatographic column is adopted, a mobile phase includes an amine-containing aqueous solution or an amine-containing phosphate, acetate or formate buffer solution and an organic solvent, and the detection wavelength is 250-350 nm. After the HPLC analysis method is performed, the detection sensitivity of the impurity that is the N-(4-(benzyloxy)benzylidene) aniline is obviously increased, the degree of separation from the main component and other impurities is good, and product quality can be effectively controlled.

Description

technical field [0001] The present invention relates to the HPLC analysis method of 4-benzyloxybenzylidene aniline. Background technique [0002] 4-Benzyloxybenzylidene-4-fluoroaniline is a raw material for the synthesis of ezetimibe and ezetimibe, and is also an important pharmaceutical intermediate. In 4-benzyloxybenzylidene-4-fluoroaniline, if the impurity 4-benzyloxybenzylidene aniline (SCR-5014) is likely to be produced during the synthesis process, the impurity will be enriched and brought into the finished drug substance , so its content needs to be controlled. The structural formulas of 4-benzyloxybenzylidene-4-fluoroaniline and 4-benzyloxybenzylideneaniline are shown in formula I and formula II respectively: [0003] [0004] There is no record in the prior art about the specific analytical method for detecting impurity 4-benzyloxybenzylidene aniline from 4-benzyloxybenzylidene-4-fluoroaniline, and select common C18 chromatographic column for use, impurity and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 王霞任晋生雷晓雪徐华倩王佳郭起
Owner NANJING SIMCERE DONGYUAN PHARM CO LTD
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