Method for separating and detecting nebivolol hydrochloride impurity by liquid phase chromatography
A technology of high performance liquid chromatography and intermediates, which is applied in the field of separation and determination of R-type and S-type optical isomers of nebivolol intermediate-4, which can solve problems such as undiscovered, reduce interference, and ensure Solubility, Quality Controlled Effects
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Embodiment 1
[0033] Instruments and Conditions
[0034] Shimadzu high performance liquid chromatography; column: Daicel OD-RH chiral column (150mm×4.6mm)
[0035] Mobile phase: (0.05mol / L potassium dihydrogen phosphate, 10% phosphoric acid to adjust pH to 3.0)-acetonitrile=85:15
[0036] Detection wavelength: 287nm; Column temperature: 25°C; Flow rate: 1.0ml / min; Injection volume: 10μl
[0037] Experimental steps:
[0038] Take (RS)-6-fluoro-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid racemate 10mg, put it in a 20ml measuring bottle, add about 2ml of methanol to dissolve, dilute with mobile phase To the scale, shake well, as the test solution;
[0039] Get need testing solution, carry out high performance liquid chromatography analysis by above-mentioned condition, record chromatogram, the result sees figure 1 .
[0040] figure 1 The chromatographic peak with a retention time of 21.967 minutes is the chromatographic peak of S-6-fluoro-3,4-dihydro-2H-1-chromene-2-carboxylic acid, an...
Embodiment 2
[0042] Instruments and Conditions
[0043] Shimadzu high performance liquid chromatography; column: Daicel OD-RH chiral column (150mm×4.6mm)
[0044] Mobile phase: (0.02mol / L potassium dihydrogen phosphate, 10% phosphoric acid to adjust pH to 3.8)-acetonitrile=80:20
[0045] Detection wavelength: 287nm; Column temperature: 25°C; Flow rate: 1.0ml / min; Injection volume: 10μl
[0046] Experimental steps:
[0047]Take (RS)-6-fluoro-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid racemate 10mg, put it in a 20ml measuring bottle, add about 2ml of methanol to dissolve, dilute with mobile phase To the scale, shake well, as the test solution;
[0048] Get need testing solution, carry out high performance liquid chromatography analysis by above-mentioned condition, record chromatogram, the result sees figure 2 . figure 2 The chromatographic peak whose retention time is 9.667 minutes is the chromatographic peak of S-6-fluoro-3,4-dihydro-2H-1-chromene-2-carboxylic acid, and the chrom...
Embodiment 3
[0050] Instruments and Conditions
[0051] Shimadzu high performance liquid chromatography; column: Daicel OD-RH chiral column (150mm×4.6mm)
[0052] Mobile phase: (0.05mol / L sodium acetate, glacial acetic acid to adjust pH to 2.5)-acetonitrile=75:25
[0053] Detection wavelength: 287nm; Column temperature: 25°C; Flow rate: 1.0ml / min; Injection volume: 10μl
[0054] Experimental steps:
[0055] Take (RS)-6-fluoro-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid racemate 10mg, put it in a 20ml measuring bottle, add about 2ml of methanol to dissolve, dilute with mobile phase To the scale, shake well, as the test solution;
[0056] Get need testing solution, carry out high performance liquid chromatography analysis by above-mentioned condition, record chromatogram, the result sees image 3 . image 3 The chromatographic peak whose retention time is 25.333 minutes is the chromatographic peak of S-6-fluoro-3,4-dihydro-2H-1-chromene-2-carboxylic acid, and the chromatographic peak ...
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