A method for separating the enantiomers of benzoylcoridone by HPLC analysis
An enantiomer and benzoylide technology, which is applied in the field of analysis and separation of benzoylcolide enantiomers by high performance liquid chromatography, which can solve the problem of small interaction differences and enantiomers. Conforms cannot be effectively separated, low stereoselectivity, etc., to achieve the effect of improving symmetry, ensuring quality controllability, and high stereoselectivity
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Embodiment 1
[0029] Instruments and Conditions
[0030] Chromatographic column: Daicel AD-H (250×4.6mm, 5.0μm)
[0031] Mobile phase: n-hexane-absolute ethanol (90:10)
[0032] Column temperature: 30°C
[0033] Flow rate: 1.0mL / min
[0034] Sample concentration: 10μg / mL
[0035] Injection volume: 2μL
[0036] Detection wavelength: 220nm
[0037] Experimental procedure
[0038] Accurately weigh (±)-benzoyl corilide 10mg, place in a 10mL volumetric flask, dissolve and dilute to the mark with n-hexane-isopropanol (90:10), shake well, and use it as the mother solution of the test sample. Precisely draw 100 μL of the mother solution of the test product and place it in a 10mL volumetric flask, adjust the volume of n-hexane-isopropanol (90:10) solution to the mark, and prepare (±)-benzoylcoridone with a concentration of 10 μg / mL Need testing solution, draw need testing solution 2 μ L and enter liquid chromatography, record chromatogram.
[0039] Experimental results: see attached figure ...
Embodiment 2
[0041] Instruments and Conditions
[0042] Chromatographic column: BC chiral AS-H (250×4.6mm, 5.0μm)
[0043] Mobile phase: n-hexane-isopropanol (90:10)
[0044] Column temperature: room temperature
[0045] Flow rate: 1.0mL / min
[0046] Sample concentration: 10μg / mL
[0047] Injection volume: 1μL
[0048] Detection wavelength: 210nm
[0049] Experimental procedure
[0050]Accurately weigh (±)-benzoyl corilide 10mg, place in a 10mL volumetric flask, dissolve and dilute to the mark with n-hexane-isopropanol (90:10), shake well, and use it as the mother solution of the test sample. Precisely draw 100 μL of the mother solution of the test product and place it in a 10mL volumetric flask, adjust the volume of n-hexane-isopropanol (90:10) solution to the mark, and prepare (±)-benzoylcoridone with a concentration of 10 μg / mL For the test solution, draw 1 μL of the test solution into the liquid chromatograph, and record the chromatogram.
[0051] Experimental results: the sepa...
Embodiment 3
[0053] Instruments and Conditions
[0054] Chromatographic column: BC chiral AS-H (250×4.6mm, 5.0μm)
[0055] Mobile phase: n-hexane-isopropanol (80:20)
[0056] Column temperature: room temperature
[0057] Flow rate: 0.8mL / min
[0058] Sample concentration: 5μg / mL
[0059] Injection volume: 5μL
[0060] Detection wavelength: 235nm
[0061] Experimental procedure
[0062] Accurately weigh (±)-benzoyl corilide 10mg, place in a 10mL volumetric flask, dissolve and dilute to the mark with n-hexane-isopropanol (80:20), shake well, and use it as the mother solution of the test sample. Precisely draw 50 μL of the mother liquor and place it in a 10mL volumetric flask, adjust the volume to the mark with the n-hexane-isopropanol (80:20) solution, and prepare (±)-benzoylcoridone test sample with a concentration of 5 μg / mL solution, absorb 5 μL of the test solution into the liquid chromatograph, and record the chromatogram.
[0063] Experimental results: the separation degree of ...
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