Separation and detection method of Baloxavir marboxil optical isomer
A technology of optical isomers and lower alcohols, applied in the field of analytical chemistry, can solve problems such as the separation and detection method of Baloxavirmarboxil optical isomers that have not been found
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Embodiment 1-9
[0064] Example 1-9: Separation and detection of Baloxavir marboxil and its enantiomers with CHIRALPAK AD chiral chromatography column
Embodiment 1
[0066] Instruments and Conditions
[0067] Chromatographic column: CHIRALPAK AD-3 150*4.6mm, 3μm;
[0068] Detector: DAD (ultraviolet detector), detection wavelength 210nm;
[0069] Flow rate: 0.8mL / min;
[0070] Column temperature: 35°C;
[0071] Injection volume: 5 μL;
[0072] Mobile Phase A: n-Hexane
[0073] Mobile Phase B: Ethanol (0.3% TFA, V / V)
[0074] Elution ratio: mobile phase A: mobile phase B = 70:30 (V:V)
[0075] Running time: 40min;
[0076] Diluent / blank solution: ethanol:n-hexane=4:1(V:V);
[0077] Experimental procedure
[0078] Take about 20 mg of Baloxavir marboxil configuration RS+RR sample, accurately weigh it into a 10mL brown measuring bottle, dissolve it with a diluent and dilute to the mark, shake well, and use it as configuration RS+RR solution.
[0079] Take about 20 mg of Baloxavir marboxil configuration SR+SS sample, accurately weigh it into a 10ml brown volumetric flask, ultrasonically dissolve it with a diluent and dilute to the mark,...
Embodiment 2
[0085] Instruments and Conditions
[0086] Chromatographic column: CHIRALPAK AD-3 150*4.6mm, 3μm;
[0087] Detector: DAD (ultraviolet detector), detection wavelength 210nm;
[0088] Flow rate: 1.0mL / min;
[0089] Column temperature: 35°C;
[0090] Injection volume: 5 μL;
[0091] Mobile Phase A: n-Hexane
[0092] Mobile Phase B: Ethanol (0.3% TFA, V / V)
[0093] Elution ratio: mobile phase A: mobile phase B = 70:30 (V:V)
[0094] Running time: 40min;
[0095] Diluent / blank solution: ethanol:n-hexane=4:1(V:V);
[0096] Experimental procedure
[0097] Take about 20mg of Baloxavir marboxil mixed standard sample (containing Baloxavir marboxil and its 3 optical isomers) respectively, accurately weigh it into a 10mL brown measuring bottle, dissolve it with diluent and dilute to the mark, shake well, and use it as a mixed standard sample.
[0098] Get the mixed standard sample solution of Baloxavir marboxil, carry out high-performance liquid chromatography analysis according to...
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