Method for detecting liquid phase content of ketoconazole component in compound ketoconazole ointment
The technology of compound ketoconazole and detection method is applied in the field of detection of the liquid phase content of ketoconazole components in compound ketoconazole ointment, which can solve the problems affecting the repeatability and accuracy of the measurement results, and the health injury of the detection personnel, etc. Avoid the effects of extraction effect, excellent detection effect and high precision
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[0043] The selection and optimization of the preparation step conditions of the above test solution is also one of the main reasons that the detection method of the present invention can more accurately measure the ketoconazole content in the compound ketoconazole ointment, specifically:
[0044] The content determination method of "ketoconazole cream" disclosed in the 2015 edition of "Chinese Pharmacopoeia" is as follows: take 2.5g of this product, weigh it accurately, put it in a beaker, add methanol-chloroform (1:1) 20ml, place Shake in a water bath at 80°C to dissolve ketoconazole, quantitatively transfer to a 50ml volumetric flask with methanol-chloroform (1:1), let cool, dilute to the mark with methanol-chloroform (1:1), shake After cooling in an ice bath for 1 hour, filter, take the filtrate and place it at room temperature, as the test solution, accurately measure 10 μl, inject it into the liquid chromatograph, and record the chromatogram; take another appropriate amoun...
Embodiment 1
[0060] Embodiment 1 Compound ketoconazole ointment ketoconazole component HPLC content determination method established by the present invention
[0061] Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; 0.02mol / L tetrabutylammonium hydrogen sulfate is used as mobile phase A, methanol is used as mobile phase B, and gradient washing is carried out according to the procedure in the table below. off; the detection wavelength is 240nm. The number of theoretical plates is not less than 2000 based on the peak of ketoconazole.
[0062] time (min)
[0063] test methods:
[0064] Get 5g of compound ketoconazole ointment, accurately weighed, put in a 50ml measuring bottle, add methanol-chloroform (1:1) 20ml, ultrasonic 30min makes ketoconazole dissolve, let cool, add methanol-chloroform (1:1) : 1) dilute to scale, shake up, filter immediately after cooling in an ice bath for 1 hour, get the continued filtrate and pla...
Embodiment 2
[0115] Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; 0.02mol / L tetrabutylammonium hydrogen sulfate is used as mobile phase A, methanol is used as mobile phase B, and gradient washing is carried out according to the procedure in the table below. off; the detection wavelength is 240nm. The number of theoretical plates is not less than 2000 based on the peak of ketoconazole.
[0116] time (min)
Mobile phase A(%)
Mobile phase B(%)
0
70
30
7
60
40
10
60
40
13
50
50
18
50
50
19
70
30
22
70
30
[0117] Determination method: take 5g of compound ketoconazole ointment, accurately weigh it, put it in a 50ml measuring bottle, add 20ml of methanol-chloroform (1:1), shake it in a water bath at 80°C to dissolve the ketoconazole, let it cool, Dilute to the mark with methanol-chloroform (1:1), shake well, filter immediately af...
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Abstract
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