HPLC analytic method for Nicorandil-related substances

An analysis method and nicorandil technology, applied in the direction of analysis materials, material separation, measurement devices, etc., can solve the problems of physical damage to the experimenter, pollution of the environment, long analysis time, etc., so as to reduce the collection time and economic cost. Reduced, reproducible effect

Inactive Publication Date: 2017-05-31
XIAN KAIBEI NAITE INTELLIGENT ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has realized the analysis to the related substance of nicorandil, but existing problem is: the tetrahydrofuran in mobile phase is highly toxic, has damage to experimenter's body, pollutes environment; Triethylamine is a volatile salt, It is also harmful to the experimenters and the environment; the analysis time is long, and the main peak (nicorandil) peak time is about 18 minutes. According to industry practice, when analyzing related substances in the sample, the collection time of a single sample is at least 3 times the time of the main peak peak. times, that is, a single sample collection time of at least 54min

Method used

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  • HPLC analytic method for Nicorandil-related substances
  • HPLC analytic method for Nicorandil-related substances
  • HPLC analytic method for Nicorandil-related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1.1 Preparation of sample solution: Use the mobile phase as the solvent, accurately weigh an appropriate amount of Nicorandil for injection, prepare a 1.0mg / ml sample solution, and then filter it with a 0.45um filter membrane as the Nicorandil sample solution. Precisely pipette 1ml of the above-mentioned nicorandil sample solution into a 100ml volumetric flask, add mobile phase to dissolve, make up to volume, shake well and use as self-control solution.

[0020] 1.2 Chromatographic conditions: The chromatographic column is a C18 silica gel column (Agilent, Zorbax Eclipse, 250㎜×4.6㎜, 5um), and the mobile phase is a mixed solution of buffer solution, methanol and tetrahydrofuran (buffer solution: methanol: tetrahydrofuran = 98.5:0.5:1.0 V / V / V), wherein the composition of the buffer solution is trifluoroacetic acid and triethylamine, the pH range is adjusted to 6.0 with triethylamine, and the volume fraction of trifluoroacetic acid is 0.01%; the column temperature is 35°C,...

Embodiment 2

[0024] 2.1 Sample solution preparation: the same preparation as the sample solution under Example 1.

[0025] 2.2 Chromatographic conditions: The chromatographic column is a C18 silica gel column (Agilent, Zorbax Eclipse, 250㎜×4.6㎜, 5um), and the mobile phase is a mixed solution of buffer solution, methanol and tetrahydrofuran (buffer solution: methanol: tetrahydrofuran = 98.5:0.5:1.0 V / V / V), wherein the composition of the buffer solution is trifluoroacetic acid and triethylamine, the pH range is adjusted to 6.2 with triethylamine, and the volume fraction of trifluoroacetic acid is 0.01%; the column temperature is 30°C, and the flow rate is 1.0ml / min, the detection wavelength is 254nm, and the injection volume is 20ul.

[0026] 2.3 Sample injection: Take the sample solution under item 2.1 and inject according to the chromatographic conditions under item 2.2.

[0027] 2.4 Results: After the elution is complete, the chromatogram of the sample solution is obtained. Results Th...

Embodiment 3

[0029] 3.1 Sample solution preparation: the same as the sample solution preparation under Example 1.

[0030] 3.2 Chromatographic conditions: The chromatographic column is a C18 silica gel column (Agilent, Zorbax Eclipse, 250㎜×4.6㎜, 5um), and the mobile phase is a mixed solution of buffer solution, methanol and tetrahydrofuran (buffer solution: methanol: tetrahydrofuran = 98.5:0.5:1.0 V / V / V), wherein the composition of the buffer solution is trifluoroacetic acid and triethylamine, the pH range is adjusted to 5.8 with triethylamine, and the volume fraction of trifluoroacetic acid is 0.01%; the column temperature is 40°C, and the flow rate is 1.0ml / min, the detection wavelength is 254nm, and the injection volume is 20ul.

[0031] 3.3 Sample injection: Take the sample solution under item 3.1 and inject according to the chromatographic conditions under item 3.2.

[0032] 3.4 Results: After the elution is complete, the chromatogram of the sample solution is obtained. As a resul...

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Abstract

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to an HPLC analytic method for Nicorandil-related substances. The HPLC analytic method is characterized in that a stationary phase is a reversed-phase column of carbon octadecyl silane, and a moving phase is a mixed solution of a buffer solution, methyl alcohol and tetrahydrofuran. The HPLC analytic method is quick, simple and accurate, is good in repeatability and suitable for control and stability study of the related substances, lays a foundation for formulating quality standards of the related substances, and makes drug quality control and medication safety possible. Through scaling down organic solvents and volatile salt, which have high toxicity, the acquisition time is shortened, the economic cost is lowered, the HPLC analytic method is suitable for large-scale production, and meanwhile, harms to experimenters and environments are reduced.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to an HPLC assay method for related substances of nicorandil. Background technique [0002] Nicorandil, also known as Nicotin and Nicotinate, belongs to nitrate ester compounds. It is the only drug for the treatment of coronary heart disease and angina pectoris with dual effects among the cardiovascular system drugs currently on the market. It not only has the effects of nitrates to expand coronary blood vessels, continuously increase coronary blood flow, and prevent coronary spasm, but also prevents the dissociation of intracellular calcium ions and increases the permeability of cell membranes to potassium ions. In addition, it also has the effect of inhibiting platelet aggregation and preventing the formation of thrombus. Its structural formula is as follows: [0003] [0004] In accordance with the ICH (International Council for Harmonization of Technical R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 吕文虎
Owner XIAN KAIBEI NAITE INTELLIGENT ENG
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