High performance liquid chromatography method for determining related substances in bifonazole bulk drug

A high-performance liquid chromatography and bifonazole technology, applied in the field of analysis and detection, can solve problems such as poor separation reproducibility, unstable analysis methods, and poor peak shape of bifonazole

Pending Publication Date: 2022-03-29
纳谱分析技术(苏州)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the challenges in the current Chinese Pharmacopoeia method are as follows: the analytical method is unstable, which is reflected in the peak shape and retention time of bifonazole: 1) Different types of C18 reverse-phase chromatographic columns have the same mobile phase preparation method, and bifonazole 2) The same chromatographic method with the same bottle of mobile phase, continuous injection, poor reproducibility of bifonazole; 3) The same mobile phase preparation method for the same chromatographic column, but the separation reproducibility of different water sources bad
The traceability analysis is as follows: 1) The imidazole functional group in the bifonazole structure can be protonated under acidic conditions, so it is positively charged and can interact with the silanol on the surface of the silica-based chromatographic filler; 2) The mobile phase uses pure In the water system, due to uncontrolled pH, the charge state of silanol and bifonazole on the surface of the stationary phase is unstable, thus affecting the stability of peak shape and retention time

Method used

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  • High performance liquid chromatography method for determining related substances in bifonazole bulk drug
  • High performance liquid chromatography method for determining related substances in bifonazole bulk drug
  • High performance liquid chromatography method for determining related substances in bifonazole bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] On the basis of the "China Pharmacopoeia" 2020 (two), this example uses a phosphate buffer system, the same mobile phase, and the different types of reverse phase C18 columns are tested, and the high performance liquid chromatography is like figure 1 As shown, the test results are shown in Table 1.

[0056] The test conditions for high performance liquid chromatography are as follows:

[0057] Column: There is a pinned single point bond C18 (4.6 × 250 mm, 5 μm);

[0058] The endless single-point bonded side chain protection C18 (4.6 × 250 mm, 5 μm);

[0059] There is a top of the multi-point bond C18 (4.6 × 250mm, 5 μm);

[0060] Mobile phase: 84 / 1 / 15V / V / V methanol / tetrahydrofuran / 10 mM phosphate dihydroxymethymmonium, pH3.0;

[0061] Flow speed: 1.0ml / min;

[0062] Column temperature: 25 ° C;

[0063] Number of injections: 10μL;

[0064] Test wavelength: UV 254 nm;

[0065] Sample: Trouble solution.

[0066] Table 1

[0067]

[0068] As can be seen from Table...

Embodiment 2

[0070] Based on the "China Pharmacopoeia" 2020 (two), this example uses a phosphate buffer system, the same mobile phase, and the different manufacturers in reverse phase C18 column for testing, high performance liquid chromatography figure 2 As shown, the test results are shown in Table 2.

[0071] The test conditions for high performance liquid chromatography are as follows:

[0072] Column: There is a pinned single point bond C18 (4.6 × 250 mm, 5 μm);

[0073] Imported brand Kromasil 100-5-C18 (4.6 × 250mm, 5μm);

[0074] Mobile phase: 84 / 1 / 15V / V / V methanol / tetrahydrofuran / 10 mM phosphate dihydroxymethymmonium, pH3.0;

[0075] Flow speed: 1.0ml / min;

[0076] Column temperature: 25 ° C;

[0077] Number of injections: 10μL;

[0078] Test wavelength: UV 254 nm;

[0079] Sample: Trouble solution.

[0080] Table 2

[0081]

[0082] It can be seen from Table 2 that use a phosphate buffer system, with 84 / 1 / 15 V / V / V methanol / tetrahydrofuran / 10 mM phosphate (pH 3.0...

Embodiment 3

[0084] On the basis of the "China Pharmacopoeia" 2020 (two), this example uses acetate buffer system, the same mobile phase, different types of reverse phase C18 columns for testing, high performance liquid chromatography image 3 As shown, the test results are shown in Table 3.

[0085] The test conditions for high performance liquid chromatography are as follows:

[0086] Column: There is a pinned single point bond C18 (4.6 × 250 mm, 5 μm);

[0087] The endless single-point bonded side chain protection C18 (4.6 × 250 mm, 5 μm);

[0088] There is a top of the multi-point bond C18 (4.6 × 250mm, 5 μm);

[0089] Mobile phase: 84 / 1 / 15V / v / v methanol / tetrahydrofuran / 20 mM ammonium acetate, pH 5.2;

[0090] Flow speed: 1.0ml / min;

[0091] Column temperature: 25 ° C;

[0092] Number of injections: 10μL;

[0093] Test wavelength: UV 254 nm;

[0094] Sample: Trouble solution.

[0095] table 3

[0096]

[0097] It can be seen from Table 3 that use acetate buffer system, with 84...

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Abstract

The invention provides a high performance liquid chromatography method for determining related substances in a bifonazole bulk drug. The high performance liquid chromatography method for determining the related substances in the bifonazole bulk drug comprises the following steps: 1) dissolving a to-be-determined sample of the bifonazole bulk drug in a mobile phase, and filtering to obtain a to-be-determined solution; and 2) measuring the standard solution and the solution to be measured by using a high performance liquid chromatography by using a mixed solution of a buffer solution and a solvent as a mobile phase to obtain a standard curve, and analyzing the contents of the bifonazole and the related substances in the solution to be measured according to the standard curve. The high performance liquid chromatography method disclosed by the invention is good in separation selectivity, symmetrical in peak shape, linear in quantitative curve, good in repeatability, and stable in retention time, separation degree and signal response value.

Description

Technical field [0001] The present invention belongs to the field of analysis and detection, and involves a highly efficient liquid chromatography method for determining the substance in the phenylphenazole. Background technique [0002] Benzazole, chemically named 1- (ρ, α-diphenylbenzyl) imidazole, is an imidazole derivative, a halogen-free imidazole antifungal, odorless, in methanol or anhydrous ethanol Skethes, almost insoluble in water, the pharmacological effect is: biphenzazole has the efficacy of broad-spectrum anti-skin sputum, yeast, filamentous bacteria, and double phase fungi, and has strong antibacterial activity, for bran Sputum and Gram-positive Soclas are also effective, animal experimental skin phenolosis has good effect; its antibacterial spectrum is wide, the effect of 90% of pathogenic fungi can inhibit a variety of skin fungi (such as furcums, Small spores Bacillus (ChemicalBook, such as monococcus, bottle yeast, optical proposed yeast), mold (such as Aspergi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 张永梅杨洋刘晓东
Owner 纳谱分析技术(苏州)有限公司
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