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Detection method and application of 3-quinuclidinone hydrochloride

A quinuclidine hydrochloride and detection method technology, applied in the field of medicinal chemistry, can solve the problems of complicated operation, low recovery rate and precision, poor stability and repeatability, etc., and achieves good repeatability, remarkable recovery rate, good stability

Active Publication Date: 2020-06-09
北京鑫开元医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The existing detection method for this impurity is complex in operation, its stability and repeatability are poor, and the recovery rate and precision are low. Therefore, the present invention has established a new method with high stability, good repeatability and practicality. Strong, simple and convenient method for quantitative detection of 3-quinuclidinone hydrochloride in penehyclidine hydrochloride

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  • Detection method and application of 3-quinuclidinone hydrochloride
  • Detection method and application of 3-quinuclidinone hydrochloride
  • Detection method and application of 3-quinuclidinone hydrochloride

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Embodiment 1

[0030] Embodiment 1-in order to carry out quantitative detection to the 3-quinuclidone hydrochloride in penhyclidine hydrochloride, the present invention proposes a kind of detection method of 3-quinuclidone hydrochloride, comprises the steps:

[0031] Prepare the sample solutions to be tested: 3-quinuclidone hydrochloride reference substance solution and penhyclidine hydrochloride test solution, and draw equal amounts into the high-efficiency chromatograph for determination. The determination conditions include: chromatographic column: benzene Base column, column length (4.4~4.8)mm×300mm, packing particle size 4~6μm; mobile phase is 0.2~1% difluoroacetic acid solution: acetonitrile=95:5, flow rate is 0.2~0.5ml / min, column temperature 25-30°C, the detector is a differential refraction detector, and the temperature of the detection cell of the differential refraction detector is 35-45°C.

Embodiment 2

[0032] Embodiment 2-a kind of detection method of 3-quinuclidone hydrochloride, comprises the steps:

[0033] (1) prepare 3-quinuclidone hydrochloride reference substance solution:

[0034] Weigh 3-quinuclidone hydrochloride reference substance and mix it with the mobile phase, the mobile phase is 0.2% difluoroacetic acid solution: acetonitrile=95:5, g / L by mass volume ratio, 3-quinuclidone salt Salt reference substance: the ratio of the mobile phase is 0.01:1000, and it is prepared as a 3-quinuclidone hydrochloride reference substance solution for use;

[0035] (2) preparation penhyclidine hydrochloride need testing solution

[0036] Take penehyclidine hydrochloride sample and mix with mobile phase, mobile phase is 0.2% difluoroacetic acid solution: acetonitrile=95:5, by mass volume ratio g / L, penhyclidine hydrochloride sample: the ratio of mobile phase is 0.01:1, prepared into penehyclidine hydrochloride test solution, stand-by;

[0037] (3) Draw the reference substance s...

Embodiment 3

[0038] Embodiment 3-a kind of detection method of 3-quinuclidone hydrochloride, comprises the steps:

[0039] (1) prepare 3-quinuclidone hydrochloride reference substance solution:

[0040] Weigh 3-quinuclidone hydrochloride reference substance and mix it with mobile phase, mobile phase is 1% difluoroacetic acid solution: acetonitrile=95:5, g / L by mass volume ratio, 3-quinuclidone salt Salt reference substance: the ratio of the mobile phase is 0.1:1000, and it is prepared as a 3-quinuclidone hydrochloride reference substance solution for use;

[0041] (2) preparation penhyclidine hydrochloride need testing solution

[0042] Weigh penhyclidine hydrochloride sample and mix with mobile phase, mobile phase is 1% difluoroacetic acid solution-: acetonitrile=95:5, by mass volume ratio g / L, penhyclidine hydrochloride sample: the ratio of mobile phase 0.1:1, prepared into penehyclidine hydrochloride test solution, stand-by;

[0043](3) Draw the reference substance solution and the n...

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Abstract

The invention provides a detection method of 3-quinuclidinone hydrochloride. According to the method, a to-be-detected sample solution is prepared respectively, an equal amount of the to-be-detected sample solution is sucked and injected into a high-performance chromatograph for determination under the determination conditions that a chromatographic column is a phenyl column, the column length is(4.4-4.8) mm*300mm, and the filler particle size is 4-6 mu m; the ratio of the mobile phase 0.2-1% difluoroacetic acid solution to acetonitrile is 95: 5, the flow rate is 0.2-0.5 ml / min, the column temperature is 25-30 DEG C, and the detector is a differential refraction detector. The method provided by the invention realizes the quantitative detection of 3-quinuclidinone hydrochloride in penehyclidine hydrochloride, has the advantages of good stability, good repeatability, high precision and significant recovery rate, and in the actual detection process, the RSD of a determination result of the solution stability within 8 hours is 0.8%; the RSD of the repeatability is 0.18%; the RSD of the precision is 0.25%, the recovery rate is higher than 99.0%, the applicability is high, and the operation is simpler and more convenient.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a detection method and application of 3-quinuclidone hydrochloride. Background technique [0002] Impurities in drugs are usually residues of starting materials and by-products or degradation products, which have a great impact on pharmacodynamics, pharmacokinetics, and pharmacology and toxicology. How to accurately quantify impurities has become a key factor in controlling impurities in drugs. prerequisites. Effective and accurate impurity detection method can accurately quantify impurities and effectively control impurities. [0003] Penehyclidine hydrochloride, chemical name: 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine hydrochloride. The chemical formula is: [0004] [0005] Penehyclidine hydrochloride is a highly selective anticholinergic drug, and its injection is a new anticholinergic drug created by Youji jointly developed by Chengdu Lisite Ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/74
CPCG01N30/02G01N30/06G01N30/54G01N30/74
Inventor 赵宇夏中宁
Owner 北京鑫开元医药科技有限公司
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