Gas chromatography detection method of dicyclohexylamine in favipiravir
A technology of dicyclohexylamine and gas chromatography, which is applied in the field of gas chromatography detection of dicyclohexylamine content in favipiravir, can solve the problems of low recovery rate of dicyclohexylamine, achieve good reproducibility and eliminate reaction Adsorption, accurate results
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[0031] Chromatographic conditions: Agilent HP-5 gas chromatography column, the stationary phase is (5%-phenyl)-methylpolysiloxane, the specification: 30m×0.53mm×5.00μm, the flow rate is 4.0ml / min, and the split ratio is 1 : 1; temperature programmed to 40°C for 3 minutes, 10°C / min to 200°C, and hold for 5 minutes; 20°C / min to 220°C, and hold for 10 minutes;
[0032] The diluent is N,N dimethylacetamide;
[0033] Preparation of linear dicyclohexylamine solution: Take 16 mg of dicyclohexylamine, accurately weigh it and set it in a 100ml volumetric flask, dissolve it with a diluent and dilute to the mark, mix well; accurately transfer 2.0ml into a 100ml volumetric flask, and dilute to Scale, mix well; then pipette 2.0ml, 5.0ml, 8.0ml, 10.0ml, 15.0ml precisely, place them in four 20ml volumetric flasks, dilute to the mark with diluent, mix well; get 0.32, 0.80, 1.28 , 1.60, 2.40, 3.20 μg / ml linear solution; precisely pipette 1.0ml of each linear solution into the injection bottle...
Embodiment 1
[0055] Chromatographic conditions: Agilent HP-5 gas chromatography column, the stationary phase is (5%-phenyl)-methylpolysiloxane, the specification: 30m×0.53mm×5.00μm, the flow rate is 4.0ml / min, and the split ratio is 1 : 1; temperature programmed at 40°C for 3 minutes, 10°C / min to 200°C, and held for 12 minutes; diluent: N,N dimethylacetamide;
[0056] Dicyclohexylamine control solution: prepare 1.6 μg / ml dicyclohexylamine solution, take 1.0ml into the sample bottle, then add 100μl of 30% sodium hydroxide solution and mix well;
[0057] Sample solution: Weigh 80mg of favipiravir sample and add 1.0ml of diluent N,N dimethylacetamide to dissolve, then add 100μl of 30% sodium hydroxide solution and mix well. Clear liquid injection;
[0058] Dicyclohexylamine sample recovery experiment: Weigh 80 mg of favipiravir sample, add 1.0ml of dicyclohexylamine control solution to dissolve; then add 100 μl of 30% sodium hydroxide solution and mix well. After shaking, a large amount of s...
Embodiment 2
[0060] Embodiment 2: compare the volume of adding lye, place time, place temperature parameter comparison
[0061] Chromatographic conditions Agilent HP-5 gas chromatography column, the stationary phase is (5%-phenyl)-methylpolysiloxane, the specification: 30m×0.53mm×5.00μm, the flow rate is 4.0ml / min, and the split ratio is 1: 1. Program temperature rise to 40°C for 3 minutes, 10°C / min to 200°C and hold for 12 minutes; diluent: N,N dimethylacetamide;
[0062] The first group: dicyclohexylamine control solution: prepare 1.6μg / ml dicyclohexylamine solution; take 1.0ml of this solution, add 60mg solid NaOH, seal and shake;
[0063] Sample solution: Weigh 80mg of favipiravir sample, add 1.0ml N,N dimethylacetamide to dissolve; add 60mg solid NaOH, seal and shake;
[0064] Dicyclohexylamine sample recovery solution: weigh 80 mg of favipiravir sample, add 1.0ml of dicyclohexylamine reference solution to dissolve; add and weigh 60mg of solid NaOH, seal and shake.
[0065] The seco...
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