Analysis method for related substances in amiodarone hydrochloride bulk drugs

A technology for amiodarone hydrochloride and related substances, which is applied in the field of analysis of related substances in amiodarone hydrochloride raw materials, can solve problems such as inability to obtain effective separation, and achieve the effects of small quantitative limit, high sensitivity and increased accuracy

Active Publication Date: 2019-09-20
合肥拓锐生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] With reference to the chromatographic conditions of the related substances in the ChP2015 two-part amiodarone hydrochloride quality standard, plus the relevant starting materials, intermediates and potential process impurities in the synthetic route, a preliminary investigation of the detection methods of the related substances was carried out, and it was found that some impurities were inconsistent with each other. Can be effectively separated, so it is necessary to establish a suitable analytical method to achieve accurate and effective detection and monitoring of related substances in amiodarone hydrochloride

Method used

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  • Analysis method for related substances in amiodarone hydrochloride bulk drugs
  • Analysis method for related substances in amiodarone hydrochloride bulk drugs
  • Analysis method for related substances in amiodarone hydrochloride bulk drugs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Establishment of Analytical Method for Related Substances in Amiodarone Hydrochloride API

[0031] method one)

[0032] Referring to the chromatographic conditions of the related substances in the ChP2015 Part II amiodarone hydrochloride quality standard, plus the relevant starting materials, intermediates and potential process impurities in the synthetic route, a preliminary investigation of the detection methods of the related substances was carried out.

[0033] a. Chromatographic conditions

[0034] Chromatographic column: Welch Ultimate AQ-C18, 4.6mm×150mm, 5μm;

[0035] Mobile phase: buffer solution (take 3.0ml of glacial acetic acid, add 800ml of water, adjust the pH to 4.9 with ammonia water, then dilute to 1000ml with water)-methanol-acetonitrile (30:30:40);

[0036] Flow rate: 1.0ml / min; Column temperature: 35°C; Detection wavelength: 240nm; Injection volume: 10μl.

[0037] b. Test procedure

[0038] Impurities A, D, E, F, G, 7, 9 and 11 mother liquors: We...

Embodiment 2

[0185] Related substances (1) Determination of impurities A, B, C, D, E, G, 9, 13, 16 and other unknown impurities

[0186] Determine according to high-performance liquid chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0512).

[0187] a. Chromatographic conditions A

[0188] Use octadecylsilane bonded silica gel as filler (Welch AQ-C18, 4.6×150mm, 5μm);

[0189] Use acetic acid buffer (take 3.0ml of glacial acetic acid, add 800ml of water, adjust the pH value to 5.95 with ammonia water, add water to 1000ml)-organic phase (methanol-acetonitrile (30:40)) (49:51) as mobile phase A; Methanol-acetonitrile (30:40) is mobile phase B;

[0190] The flow rate is 1.0ml per minute; the detection wavelength is 238nm; the column temperature is 33°C;

[0191] Use acetic acid buffer (take 3.0ml of glacial acetic acid, add 800ml of water, adjust the pH value to 4.85 with ammonia water, add water to 1000ml)-organic phase (methanol-acetonitrile (30:40)) (49:51) as the di...

Embodiment 3

[0205] Related substances (1) Determination of impurities A, B, C, D, E, G, 9, 13, 16 and other unknown impurities

[0206] Determine according to high-performance liquid chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0512).

[0207] a. Chromatographic conditions A

[0208] Use octadecylsilane bonded silica gel as filler (Welch AQ-C18, 4.6×150mm, 5μm);

[0209] Use acetic acid buffer (take 3.0ml of glacial acetic acid, add 800ml of water, adjust the pH value to 6.05 with ammonia water, add water to 1000ml)-organic phase (methanol-acetonitrile (30:40)) (51:49) as mobile phase A; Methanol-acetonitrile (30:40) is mobile phase B;

[0210] The flow rate is 1.0ml per minute; the detection wavelength is 242nm; the column temperature is 37°C;

[0211] Use acetic acid buffer (take 3.0ml of glacial acetic acid, add 800ml of water, adjust the pH value to 4.95 with ammonia water, add water to 1000ml)-organic phase (methanol-acetonitrile (30:40)) (51:49) as the di...

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Abstract

The invention discloses an analysis method for related substances in amiodarone hydrochloride bulk drugs, and relates to the technical field of chemical drug analysis methods. High performance liquid chromatograph is used carry out analysis according to chromatogram conditions A and B respectively and then in a combined way; the chromatogram conditions A and B include a chromatographic column of Welch Ultimate AQ-C18, a mobile phase A in which the proportion of an acetic acid-ammonium acetate buffer solution to a methanol and acetonitrile mixed solution is 49-51vt% to 51-49vt%, a mobile phase B in which the ratio of methanol to acetonitrile is 30vt% to 40vt%, and the detection wavelength for gradient wash out is 240+ / -2nm; the ratio of methanol to acetonitrile in the methanol and acetonitrile mixed solution is 30vt% to 40vt%; the pH value of the acetic acid-ammonium acetate buffer solution in the chromatogram condition A is 5.95-6.05; and the pH value of the acetic acid-ammonium acetate buffer solution in the chromatogram condition B is 4.85-4.95. Thus, more impurities can be detected, and related substances in amiodarone hydrochloride can monitored rapidly, effectively and accurately.

Description

technical field [0001] The invention relates to the technical field of analytical methods for chemical drugs, in particular to an analytical method for related substances in amiodarone hydrochloride raw materials. Background technique [0002] Amiodarone hydrochloride, the chemical name is 2-butyl-3-benzofuryl-4-[2-(diethylamino)ethoxy]-3,5-diiodophenyl ketone salt acid salt, the molecular formula is C 25 h 29 I 2 NO 3 HCl, its structural formula is as follows: [0003] [0004] Amiodarone hydrochloride is currently one of the most clinically used antiarrhythmic drugs, which can selectively expand coronary blood flow, reduce myocardial oxygen consumption, slow down heart rate, reduce atrioventricular conduction velocity and β-receptor Blockers have a similar effect. For supraventricular and ventricular tachycardia, paroxysmal atrial flutter and fibrillation, pre-excitation syndrome, also for intractable paroxysmal tachycardia, chronic coronary insufficiency and angi...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陆文通戴德标单胜男耿爽
Owner 合肥拓锐生物科技有限公司
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