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Method for simultaneous detection of hydroxychloroquine side chains, raw materials and intermediates by gas chromatography

A hydroxychloroquine side chain, gas chromatography technology, applied in the field of drug analysis, can solve the problems of no conjugation effect ultraviolet absorption, reducing the quality of hydroxychloroquine, clinical efficacy, impact, etc.

Active Publication Date: 2018-04-10
SHANGHAI INST OF TECH
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Problems solved by technology

There are 7 kinds of raw materials and intermediates involved in the synthetic route (formula III) of a kind of hydroxychloroquine side chain announced by Chinese patent (publication number: CN 104803859 A), which are respectively ethylamine (formula 1), xylene (formula 5), ethylamine ethanol (formula 2), chloropentyl ketone (formula 4), ethylamine diethanolamine (formula 3) and aminopentanone (formula 6), the remaining amount of raw material and incomplete intermediate in the reaction High will lead to low purity of the target product, and will affect the yield of synthetic hydroxychloroquine with 4,7-dichloroquinoline in the later stage, thereby reducing the quality and clinical efficacy of hydroxychloroquine
[0006] From the structural formula of the side chain of hydroxychloroquine, it can be seen that there is no conjugation effect and obvious ultraviolet absorption, and it is difficult to analyze it by liquid chromatography, which is generally simple, convenient and cost-effective

Method used

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  • Method for simultaneous detection of hydroxychloroquine side chains, raw materials and intermediates by gas chromatography
  • Method for simultaneous detection of hydroxychloroquine side chains, raw materials and intermediates by gas chromatography
  • Method for simultaneous detection of hydroxychloroquine side chains, raw materials and intermediates by gas chromatography

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Embodiment 1

[0034] (1) Chromatographic conditions and system adaptability test The chromatographic column is DB-624 cross-linked capillary column (30m×0.53mm.i.d, 3.0μm); 200°C, store for 10min; the temperature of the injection port is 300°C; the carrier gas is nitrogen; the detector is a hydrogen flame ionization detector (FID), and the detector temperature is 310°C; the flow rate is 3.0mL / min, and the split ratio is 30: 1. The separation degree of hydroxychloroquine side chain, ethylamine, ethylaminoethanol, ethylaminediethanolamine, chloropentylone, xylene, aminopentanone, and ethanol should be greater than 1.5;

[0035] (2) Preparation of mixed reference substance solution Get ethylamine ethanol, xylene, chloropentanone, ethylamine diethanolamine, aminopentanone, ethylamine, hydroxychloroquine side chain (pure product, batch number: Y023-150101, from Shanghai Zhongxi Sanwei Pharmaceutical Co., Ltd.) appropriate amount, accurately weighed respectively, put in the same measuring bottle,...

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Abstract

The invention belongs to the technical field of drug analysis and particularly relates to a method for simultaneous detection of hydroxychloroquine side chains, raw materials and intermediates by gaschromatography. The method can simultaneously determine the hydroxyl side chains, ethylamine, xylene, ethylamine ethanol, chloropentanone, ethylamine diethanolamine, amino pentanone and ethanol, and the specificity, linearity, range, precision, detection line, and accuracy are in line with the requirements of the verification guiding principles for quality standard analysis methods of traditionalChinese medicines in Chinese Pharmacopoeia 2015 Edition Volume IV. The method aims to provide a technical basis for the detection and monitoring of the synthesis process of the hydroxychloroquine sidechains.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for simultaneously detecting hydroxychloroquine side chains, raw materials and intermediates thereof by gas chromatography. Background technique [0002] Hydroxychloroquine (formula I), chemical name is 7-chloro-4-[5-(N-ethyl-N-2-hydroxyethyl-2-pentyl] aminoquinoline, is a kind of 4-aminoquinoline Drugs, which were first used clinically for the treatment of malaria parasites, are now widely used in the treatment of discoid lupus erythematosus and systemic lupus erythematosus, and are also the first choice for the treatment of rheumatoid arthritis. In addition, in immunosuppression and anti-inflammatory response There are also applications in other aspects. [0003] [0004] Hydroxychloroquine is made by 4,7-dichloroquinoline and 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine through Fisher synthesis reaction, wherein 5-(N-ethyl -N-2-hydroxyethylamine)-2-penty...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 黄金文胡美晨黄磊磊李英姿谢达朱阳斌王琳吴范宏
Owner SHANGHAI INST OF TECH
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