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Method of detecting impurities in penehyclidine hydrochloride

A penehyclidine hydrochloride and detection method technology, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of large operation error, inconspicuous color development, low detection sensitivity, etc., so as to improve the detection sensitivity and stabilize the analysis method. , the effect of increasing controllability

Active Publication Date: 2014-12-24
重庆科塞亚医药科技有限责任公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0009] At present, high-performance liquid chromatography (HPLC) is the first choice for the common detection method of drug impurities. However, 3-quinine ketone Ⅱ and 3-quinine alcohol Ⅲ are not retained in commonly used reversed-phase high-performance liquid chromatography columns, and they are not Ultraviolet absorption, it is difficult to detect with high performance liquid chromatography ultraviolet detector. When using evaporative light detector and differential refractive index detector, the detection sensitivity of impurities II and III is low and the reproducibility is poor
In the national drug standard WS1-(X-026)-2004Z, thin-layer chromatography is used to detect impurity III in penhyclidine hydrochloride, but the detection of thin-layer chromatography is affected by temperature, humidity, reagent type, and sampling technology. Such shortcomings as many influences, poor reproducibility, and inconspicuous color development, at the same time, the test results can only be semi-quantitative, and the operation error is large
At the same time, the standard stipulates that the detection limit of impurity III is only 0.25%, which cannot meet the increasing requirements for strict control of drug impurities.

Method used

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  • Method of detecting impurities in penehyclidine hydrochloride
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  • Method of detecting impurities in penehyclidine hydrochloride

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Experimental program
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Effect test

Embodiment 1

[0043] Main main instruments and chromatographic conditions:

[0044] TRACE GC ULTRA gas chromatograph, equipped with hydrogen flame ionization detector (FID), temperature 300 ℃, automatic sampler, Chromeleon chromatographic workstation.

[0045] Chromatographic column: Rtx?-5 Amine (30m×0.25mm, 0.5μm)

[0046] Column temperature: the initial temperature is 90°C, keep for 1 minute, then raise the temperature to 300°C at a rate of 8°C per minute, and keep for 8 minutes.

[0047] Column flow rate: 2. 5ml / min;

[0048] Inlet temperature: 190°C;

[0049] Split ratio: 4:1;

[0050] Injection volume: 2ul.

[0051] Penehyclidine hydrochloride was provided by Chongqing Xianyang Pharmaceutical Technology Co., Ltd., batch number: 110900.

[0052] The impurity II reference substance was provided by Chongqing Xianyang Pharmaceutical Technology Co., Ltd., batch number 110601.

[0053] The impurity III reference substance was purchased from Sigma, batch number MKBF3377V.

[0054] Pre...

Embodiment 2

[0060] According to the above chromatographic conditions and operation methods, the specificity, precision, linearity, detection limit and quantification limit, sample recovery rate and stability of the method were respectively verified by methodology, and the results are as follows:

[0061] (1) Specificity:

[0062] Take the solvent DMF, the solution of the test product, the solution of the impurity reference substance II, the solution of the impurity reference substance III, the mixed solution of the test product solution and the solutions of the impurity reference substance II and III, and inject the samples in sequence. The results show that the solvent has peaks with retention times of 1.370min, 2.565min, 2.939min, and 3.331min, the retention time of impurity II is 5.113min, the retention time of impurity III is 5.557min, and the retention time of penehyclidine is 14.948min, indicating that the solvent The separation degree from the impurity reference substance i...

Embodiment 3

[0095] With reference to the method of Example 1, the temperature of the injection port is investigated. The results are shown in Table 6:

[0096] Table 6 Inspection results of injection port temperature

[0097]

[0098] The above results show that when the temperature of the injection port is measured in the range of 150-230°C, the impurities II and III are well separated and accurate determination can be realized.

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Abstract

The invention discloses a method of detecting two impurities containing a quinuclidine ring in penehyclidine hydrochloride. The method adopts a gas chromatographic method to detect the contents of the impurities, namely the content of 3-quinuclidone and the content of 3-quinuclidinol. During detection, a sample of the penehyclidine hydrochloride is dissolved with an alkaline organic solvent so as to convert all the hydrochlorides into free alkalis and is dried by blowing nitrogen, and then dimethylformamide is added to prepare a sample solution to be detected; and impurity reference substances are processed as the same manner and prepared into impurity reference substance solutions. The sample solution to be detected and the impurity reference substance solutions are directly injected respectively, chromatograms are collected, and the contents of the impurities are calculated based on peak areas by an external standard method. The method of detecting the impurities has characteristics of simple and convenient operation, high sensitivity, capability of quantitative measurement, high accuracy and good reproducibility, effectively controls the product quality of the penehyclidine hydrochloride and guarantees safety and effectiveness of clinical medication.

Description

technical field [0001] The invention relates to a method for detecting impurities in medicines, in particular to a method for detecting 3-quinine ketone and 3-quinine alcohol in penehyclidine hydrochloride. [0002] Background technique [0003] Penehyclidine hydrochloride, chemical name: 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine hydrochloride. Chemical formula is [0004] [0005] This strain is a new type of selective anticholinergic drug, which can enter the brain through the blood-brain barrier. It can block the stimulant effect of acetylcholine on muscarinic receptors and nicotinic receptors in the brain; therefore, it can better antagonize the symptoms of central poisoning caused by organophosphate poisoning, such as convulsions, central respiratory and circulatory failure, and restlessness . At the same time, it also has a strong ability to block the stimulatory effect of acetylcholine on M receptors in the periphery; therefore, it can better antag...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 姚有良刘晓燕李凤君
Owner 重庆科塞亚医药科技有限责任公司
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