Method for analysis of hydroxychloroquine sulfate raw material and preparation by high performance liquid chromatography
A technology of high performance liquid chromatography and hydroxychloroquine sulfate, which is applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve the problems of low specificity and low sensitivity, and achieve the effect of overcoming low specificity
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Embodiment 1
[0023] Use octylsilane bonded silica gel as filler, use phosphate buffer solution (take 2.72g of potassium dihydrogen phosphate, put it in 1000ml of water, add 2ml of triethylamine, adjust the pH to 8.0±0.05 with 1mol of potassium hydroxide as mobile phase A, Methanol is the mobile phase B, carry out gradient elution according to the following table:
[0024] time (minutes)
Mobile Phase A (V / V)
Mobile phase B (V / V)
0～20
53→33
47→67
20～32
33
67
[0025] The detection wavelength is 254nm. The number of theoretical plates should not be less than 2000 based on the peak of hydroxychloroquine sulfate.
[0026] Get an appropriate amount of hydroxychloroquine sulfate crude drug, add solvent [mobile phase A-methanol (53:47)] to dissolve and dilute to make a solution containing 0.5 mg in every 1 ml as the test solution; accurately measure an appropriate amount, and dilute with the above-mentioned solvent Prepare a solution containi...
specific Embodiment 2
[0028] Use octylsilane bonded silica gel as the filler, and use phosphate buffer solution (take 3.12g of sodium dihydrogen phosphate, put it in 1000ml of water, add 5ml of triethylamine, adjust the pH to 8.0±0.05 with 1mol of potassium hydroxide) as the flow Phase A, acetonitrile as mobile phase B, carry out gradient elution according to the following table:
[0029] time (minutes)
Mobile Phase A (V / V)
Mobile phase B (V / V)
[0030] 0～25
60→20
40→80
25.1～40
20
80
[0031] The detection wavelength is 254nm. The number of theoretical plates should not be less than 2000 based on the peak of hydroxychloroquine sulfate.
[0032] Get an appropriate amount of hydroxychloroquine sulfate raw material, dissolve and dilute with a solvent [mobile phase A-acetonitrile (60:40)] to make a solution containing 0.5 mg in every 1 ml as the test solution; accurately measure an appropriate amount, and dilute with the above-mentioned s...
specific Embodiment 3
[0034] Use octadecylsilane bonded silica gel as filler, and use phosphate buffer solution (take 5.44g of potassium dihydrogen phosphate, put it in 1000ml of water, add 3ml of triethylamine, and adjust the pH value to 8.0± with 1mol / L potassium hydroxide solution 0.05)-methanol (60:40) is the mobile phase, and the detection wavelength is 254nm. The number of theoretical plates should not be less than 2000 based on the peak of hydroxychloroquine sulfate.
[0035] Take an appropriate amount of hydroxychloroquine sulfate crude drug, dissolve and dilute with mobile phase to make a solution containing 0.4 mg per 1 ml as the test solution; accurately measure an appropriate amount, dilute with mobile phase to make a solution containing 4 μg per 1 ml as a contrast solution . Accurately measure 20 μl each of the test solution and the control solution, inject them into the liquid chromatograph, and record the chromatograms. Calculate the content of related substances according to its o...
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