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Detection method for mexiletine hydrochloride associated substances

A technology of mexiletine hydrochloride and a detection method, which is applied in the detection field of related substances, can solve the problems of excessive concentration of the test sample, poor resolution of the main peak, low impurity sensitivity, etc., achieves a good baseline, improves column efficiency, and has high sensitivity Effect

Active Publication Date: 2019-11-05
上海葆隆生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In statutory pharmacopoeias such as the Chinese Pharmacopoeia, the British Pharmacopoeia, the European Pharmacopoeia, the United States Pharmacopoeia, and the Japanese Pharmacopoeia, there are determination methods for related substances of mexiletine hydrochloride. Disadvantages of low column efficiency or poor separation between impurity D and the main peak or low impurity sensitivity

Method used

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  • Detection method for mexiletine hydrochloride associated substances
  • Detection method for mexiletine hydrochloride associated substances
  • Detection method for mexiletine hydrochloride associated substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] (1) Chromatographic conditions:

[0070] Instrument: high performance liquid chromatography, wherein the detector is an ultraviolet detector;

[0071] Chromatographic column: the category and specification of octadecylsilane bonded silica gel column is C18, 4.6×250mm5μm;

[0072] Mobile phase: a mixed solution of sodium acetate buffer and methanol with a volume ratio of 50:50, the sodium acetate buffer is 0.1mol / L sodium acetate solution, and the pH value is adjusted to 5.8 with glacial acetic acid, and isocratic elution;

[0073] Detection wavelength: 262nm;

[0074] Flow rate: 1.0ml per minute;

[0075] Column temperature: 30°C;

[0076] Injection volume: 20 μl.

[0077] (2) Solution preparation:

[0078] Need testing solution: get this product appropriate amount, weigh accurately, dissolve with diluent (mobile phase A:mobile phase B=1; 1) and make the solution of about 10mg in every 1ml.

[0079] Impurity D positioning solution: Take an appropriate amount of th...

Embodiment 2

[0083] (1) Chromatographic conditions:

[0084] Instrument: high performance liquid chromatography, wherein the detector is an ultraviolet detector;

[0085] Chromatographic column: the category and specification of octadecylsilane bonded silica gel column is C18, 4.6×250mm5μm;

[0086] Mobile phase: mobile phase A is a mixed solution of sodium acetate buffer and methanol with a volume ratio of 90:10, the sodium acetate buffer is 0.1mol / L sodium acetate solution, and the pH value is adjusted to 5.8 with glacial acetic acid, mobile phase B For methanol, the gradient elution procedure is as follows:

[0087]

[0088] Detection wavelength: 262nm;

[0089] Flow rate: 1.0ml per minute;

[0090] Column temperature: 30°C;

[0091] Injection volume: 20 μl.

[0092] (2) Solution preparation:

[0093] System suitability solution: Weigh the appropriate amount of mexiletine hydrochloride impurities A, B, C, D, add methanol to dissolve and prepare to contain about 0.025mg of A, ab...

Embodiment 3

[0102] (1) Chromatographic conditions:

[0103] Instrument: high performance liquid chromatography, wherein the detector is an ultraviolet detector;

[0104] Chromatographic column: the category and specification of octadecylsilane bonded silica gel column is C18, 4.6×250mm5μm;

[0105] Mobile phase: mobile phase A is a mixed solution of sodium acetate buffer and methanol with a volume ratio of 90:10, the sodium acetate buffer is 0.1mol / L sodium acetate solution, and the pH value is adjusted to 5.8 with glacial acetic acid, mobile phase B For methanol, the gradient elution procedure is as follows:

[0106]

[0107] Detection wavelength: 262nm;

[0108] Flow rate: 1.0ml per minute;

[0109] Column temperature: 30°C;

[0110] Injection volume: 20 μl.

[0111] (2) Solution preparation:

[0112] Impurity stock solution: take 2.5mg of impurity (A, C, E, F, H) reference substance 12.5mg of impurity B reference substance, accurately weighed, put in six 25ml measuring bottles...

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Abstract

The invention relates to a detection method for complete separation of mexiletine hydrochloride associated substances. The method comprises the steps that by using high performance liquid chromatography, detection is conducted, wherein according to chromatographic conditions, octadecylsilane bonded silica gel is used as a filler of a chromatographic column, before feeding, a ghost peak capture column is added, a mixed solution of a sodium acetate buffer solution and methyl alcohol serves as a moving phase A in the chromatographic conditions, methyl alcohol serves as a moving phase B, and gradient elution is conducted. The detection method is high in column efficiency, high in sensitivity and high in repeatability, the degree of separation of a main peak from various impurities is high, theoperation is simple, and an effective and reliable analyzing method is provided for determining the mexiletine hydrochloride associated substances.

Description

technical field [0001] The invention relates to a method for detecting related substances of mexiletine hydrochloride. Background technique [0002] The English name of mexiletine hydrochloride is Mexiletine Hydrochloride, commonly known as slow heart rhythm. Mexiletine is a class IB antiarrhythmic drug, which can inhibit the sodium inflow of myocardial cells, reduce the depolarization speed of the 0 phase of the action potential, and shorten the effective force of Puertz's fibers. Refractory period, mainly used for chronic ventricular arrhythmia. [0003] 2,6-Dimethylphenol is reacted with monochloroacetone to produce sperm ketone, which is then hydrogenated to obtain spermine, which is then salified, refined, centrifuged, dried, pulverized, sieved, and mixed to obtain mexiletine hydrochloride. It is produced through multi-step reactions in the production process, and there may be process impurities, by-products or degradation impurities, so quality control of its related ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 张敏董真秀王木兰刘勇方香香廖荣园
Owner 上海葆隆生物科技有限公司
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