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Method for detecting methyl acetoacetate in benidipine hydrochloride

A technology of benidipine hydrochloride and methyl acetoacetate is applied in the field of detection of methyl acetoacetate in benidipine hydrochloride, and can solve the problem of low response value of methyl acetoacetate, interference of methyl acetoacetate measurement, benidipine hydrochloride Dipine is easily decomposed and other problems to achieve the effect of relieving angina pectoris, strong contraction and less side effects

Pending Publication Date: 2022-04-12
SUZHOU DAWNRAYS PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional detection methods such as methyl acetoacetate and ethyl acetoacetate are gas chromatography-solution direct sampling method at present, and the disadvantage of this method is that benidipine hydrochloride is easily decomposed when the test product is vaporized at high temperature, and a lot of impurities are produced, which is harmful to acetoacetate The determination of methyl ester causes interference, and the response value of methyl acetoacetate under this method is not high, and the detection sensitivity is low

Method used

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  • Method for detecting methyl acetoacetate in benidipine hydrochloride
  • Method for detecting methyl acetoacetate in benidipine hydrochloride
  • Method for detecting methyl acetoacetate in benidipine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0068] Instrument: SHIMADZU LC-2030C;

[0069] (1) Chromatographic conditions

[0070] Chromatographic column: Octadecylsilane bonded silica column (Waters C18, 4.6×150mm, 5μm);

[0071] Mobile phase A: 0.05mol / L potassium dihydrogen phosphate solution (adjust the pH value to 6.0 with 1mol / L potassium hydroxide solution)-methanol (volume ratio 82:18);

[0072] Mobile phase B: 0.05mol / L potassium dihydrogen phosphate solution (adjust the pH value to 3.0 with phosphoric acid)-methanol (volume ratio 41:59);

[0073] The elution program is shown in Table 1 below:

[0074] Table 1

[0075] time (min) Mobile phase A(%) Mobile phase B(%) 0 100 0 6 100 0 6.1 0 100 16 0 100 16.1 100 0 24 100 0

[0076] Detection wavelength: 210nm;

[0077] Flow rate: 1.0ml / min;

[0078] Injection volume: 20μl;

[0079] Column temperature: 30°C.

[0080] (2) Preparation of the solution

[0081] Solvent: 0.05mol / L potassium dihydrogen phosp...

Embodiment 2

[0198] Instrument: SHIMADZU LC-2030C;

[0199] Chromatographic column: C18 column, 4.6×150mm, 5μm;

[0200] Mobile phase: 0.05mol / L potassium dihydrogen phosphate solution (adjust the pH value to 5.0 with the flow rate)-methanol (volume ratio 87:13)

[0201] Detection wavelength: 210nm;

[0202] Flow rate: 1.0ml / min;

[0203] Injection volume: 20μl;

[0204] Column temperature: 30°C.

[0205] Methyl acetoacetate solution: Take about 20mg of methyl acetoacetate, put it in a 100ml measuring bottle, add mobile phase to dilute to the mark, shake well, take another 1ml, put it in a 20ml measuring bottle, add mobile phase to dilute to the mark, shake well. (10μg / ml)

[0206] Take methyl acetoacetate solution for sample injection, the spectrum is as follows Figure 5 shown.

Embodiment 3

[0208] The difference with embodiment 2 is:

[0209] Mobile phase: 0.05mol / L potassium dihydrogen phosphate solution (adjust the pH value to 6.0 with the flow rate), and the spectrum is as follows Figure 6 shown.

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Abstract

The invention relates to a method for detecting methyl acetoacetate in benidipine hydrochloride, a high performance liquid chromatograph is used for detecting the content of methyl acetoacetate in benidipine hydrochloride, and a mobile phase used in the high performance liquid chromatograph comprises a mobile phase A and a mobile phase B, the mobile phase A is a mixed solution of a first phosphate solution with a pH value of 5-8 and methanol, and the mobile phase B is a mixed solution of a second phosphate solution with a pH value of 2-4 and methanol; the detection method comprises the following steps: enabling benidipine hydrochloride to enter a high performance liquid chromatograph, and respectively introducing a mobile phase A and a mobile phase B into the high performance liquid chromatograph to detect benidipine hydrochloride. The detection method provided by the invention can effectively detect the residual quantity of methyl acetoacetate in benidipine hydrochloride, and the detection method has good specificity, quantitation limit and detection limit, linearity and range, precision, accuracy and durability.

Description

technical field [0001] The invention belongs to the technical field of chemical drug analysis, in particular to a method for detecting methyl acetoacetate in benidipine hydrochloride. Background technique [0002] Benidipine hydrochloride belongs to dihydropyridine calcium ion antagonists and is a kind of antihypertensive drug used clinically to treat patients with hypertension. Compared with other clinically used dipine drugs, it has stronger antihypertensive effect and less side effects ; At the same time, it also has a good curative effect on other indications that calcium ion antagonists are suitable for. In terms of relieving angina pectoris, benidipine hydrochloride has a relatively strong anti-coronary spasm effect, that is, the constriction effect of the coronary arteries is relatively strong, and it can be used to treat variant angina pectoris, and it is the drug of choice for patients with coronary artery spasm. [0003] Methyl acetoacetate is the starting materia...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/36G01N30/32G01N30/74
Inventor 姚益戴巍万梓龙张国成马成孝
Owner SUZHOU DAWNRAYS PHARM CO LTD
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