A kind of method for measuring tetrabutylammonium bromide content in organic medicine
A technology of tetrabutylammonium bromide and organic drugs, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unfriendly environment, low instrument penetration rate, poor specificity, etc., and avoid excessive analysis time , strong specificity, good reproducible effect
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Embodiment 1
[0050] Instruments and Conditions
[0051] High performance liquid chromatography: Agilent 1260;
[0052] Chromatographic column: Octadecylsilane bonded silica gel as filler (AichromBond-AQ C18 4.6 mm×250mm, 5μm);
[0053] The mobile phase A is the aqueous phase: 0.005mol / L tetramethylammonium hydroxide solution, the pH value is adjusted to 3.0 with phosphoric acid, and the mobile phase B is the organic phase: acetonitrile.
[0054] Elute according to the gradient elution table (see Table 1) (after 5 minutes, it is the equilibrium system stage).
[0055]
[0056] Injection volume: 20μl;
[0057] Column temperature: 30°C;
[0058] Detection wavelength: 210nm.
[0059] Experimental procedure
[0060] Take about 400 mg of the crude drug canagliflozin, accurately weigh it, put it in a 10ml volumetric flask, add acetonitrile aqueous solution (acetonitrile:water=90:10v / v, the same below) to dissolve and dilute to the mark, shake well, and serve as Test solution. Take about...
Embodiment 2
[0063] Instruments and Conditions
[0064] High performance liquid chromatography: Agilent 1260;
[0065] Chromatographic column: Octadecylsilane bonded silica gel as filler (AichromBond-AQ C18 4.6 mm×250mm, 5μm);
[0066] Mobile phase A: aqueous phase 0.005mol / L tetramethylammonium hydroxide solution, adjust the pH value to 3.0 with phosphoric acid, mobile phase B: acetonitrile;
[0067] Elute according to the gradient elution table (see Table 2) (after 5 min, it is the equilibrium system stage).
[0068]
[0069] Injection volume: 20μl;
[0070] Column temperature: 30°C
[0071] Detection wavelength: 210nm.
[0072] Experimental procedure
[0073] Take about 400mg of the crude drug of canagliflozin, weigh it accurately, put it in a 10ml volumetric flask, add an appropriate amount of tetrabutylammonium bromide solution accurately, add acetonitrile aqueous solution to dissolve and dilute to make tetrabutylammonium bromide in every 1ml 4 μg of the mixed solution, shake...
Embodiment 3
[0075] Instruments and Conditions
[0076] High performance liquid chromatography: Agilent 1260;
[0077] Chromatographic column: Octadecylsilane bonded silica gel as filler (AichromBond-AQ C18 4.6 mm×250mm, 5μm);
[0078] Mobile phase A: aqueous phase 0.005mol / L tetramethylammonium hydroxide solution, adjust the pH value to 2.0 with phosphoric acid, mobile phase B: acetonitrile;
[0079] Elute according to the gradient elution table (see Table 3) (after 5 min, it is the equilibrium system stage).
[0080]
[0081] Injection volume: 20μl;
[0082] Column temperature: 30°C.
[0083] Experimental procedure
[0084] Take about 10 mg of tetrabutylammonium bromide reference substance, accurately weigh it, put it in a 25ml volumetric flask, add acetonitrile aqueous solution to dissolve and dilute to the mark, shake well, and use it as a stock solution. Take 500mg of Empagliflozin crude drug, accurately weighed, put in a 10ml volumetric flask, accurately add 0.1ml of stock so...
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