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

Pending Publication Date: 2020-09-15
SUNSHINE LAKE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Quality control is required during the production of Baloxavir marboxil, but at present, Baloxavir marboxil is not recorded in the USP of the United States Pharmacopoeia, EP of the European Pharmacopoeia and Ch.P. Separation and detection method of optical isomers thereof

Method used

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  • Separation and detection method of Baloxavir marboxil optical isomer
  • Separation and detection method of Baloxavir marboxil optical isomer
  • Separation and detection method of Baloxavir marboxil optical isomer

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a separation and detection method of an optical isomer, and belongs to the field of analytical chemistry. The method specifically relates to separation and determination of Baloxavir marboxil and optical isomers thereof by liquid chromatography, and is characterized in that a polysaccharide derivative is used as a chiral chromatographic column of a filler, and a mixed solution of lower alkane and lower alcohol is used as a mobile phase. The method is simple, rapid and accurate.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and measuring isomers of Baloxavir marboxil by liquid chromatography. Background technique [0002] XOFLUZA (baloxavir marboxil) is an antiviral PA endonuclease inhibitor that can inhibit the initiation of mRNA synthesis and can be used to treat influenza A and B in adults and children. The chemical name of baloxavir marboxil is ({(12aR)-12-[(11S)-7,8-difluoro-6,11-dihydrodibenzo[b,e]thiapin11-yl]-6, 8-dioxo-3,4,6,8,12,12a-hexahydro-1H-[1,4]oxodiazo[3,4-c]pyrido[2,1-f][ 1,2,4] triazin-7-yl} oxy) methyl methyl carbonate, abbreviated as RS in the present invention, molecular weight is 571.55, and the molecular formula of Baloxavir marboxil is C 27 h 23 f 2 N 3 o 7 S, the chemical structure is shown in the following formula: [0003] [0004] There are 2 chiral centers in the Baloxavir marboxil molecule, and 4 optical isomers with different stere...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 范晓梅丘梅燕张琛霞赵蕾朱丽娜叶艳影栾保磊饶万兵刘国柱
Owner SUNSHINE LAKE PHARM CO LTD
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