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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

Inactive Publication Date: 2018-06-26
FOSHAN NANHAI EASTERN ALONG PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method for determining the content of "ketoconazole cream" disclosed in the 2015 edition of "Chinese Pharmacopoeia" can provide a solution to the determination of the liquid phase content of ketoconazole components in compound ketoconazole ointment to a certain extent, however, the "Ketoconazole Cream" in the Pharmacopoeia The disclosed method still has some disadvantages, which will not only affect the repeatability and accuracy of the measurement results, but also cause great harm to the health of the testing personnel

Method used

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  • Method for detecting liquid phase content of ketoconazole component in compound ketoconazole ointment
  • Method for detecting liquid phase content of ketoconazole component in compound ketoconazole ointment
  • Method for detecting liquid phase content of ketoconazole component in compound ketoconazole ointment

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Experimental program
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preparation example Construction

[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

The invention provides a method for detecting the liquid phase content of a ketoconazole component in a compound ketoconazole ointment. According to the detection method, high performance liquid chromatography is utilized to detect the liquid phase content of the ketoconazole component in the compound ketoconazole ointment. The detection method has strong specificity, short analysis time, high precision, good reproducibility and high accuracy; at the same time, by optimizing the type and ratio of a mobile phase solution, the detection method has a better detection effect. Therefore, the reproducibility and durability of the detection are improved, so that the method is more suitable for detecting the compound ketoconazole ointment, deviation of the detection result caused by operation errors is reduced, and the influence on the active ingredient extraction effect, the pollution to a laboratory environment and the damage to health of analysts are also avoided.

Description

technical field [0001] The invention relates to the field of veterinary drug analysis, in particular to a method for detecting the liquid phase content of ketoconazole components in compound ketoconazole ointment. Background technique [0002] Compound ketoconazole ointment is an external medicine for veterinary use. It belongs to antimicrobial medicine and is suitable for treating bacterial skin diseases in dogs and cats caused by fungi and anaerobic bacteria. The main ingredients are metronidazole, ketoconazole and menthol. [0003] Ketoconazole is a synthetic imidazole antifungal drug, which has antibacterial effects on systemic and superficial skin fungi (microsporum, epidermophyton and trichophyton), and can be used to prevent and treat skin fungal infections. [0004] The content detection method of compound ketoconazole ointment in the current national standard (i.e. "Compilation of National Standards for Veterinary Drugs - National Standards for Raising Local Standar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34
CPCG01N30/02G01N30/34
Inventor 陶映娴林孝崇焦伟丽寇贺红赵奉君倪凯燕向聪李莉
Owner FOSHAN NANHAI EASTERN ALONG PHARMA CO LTD
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