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Method of detecting impurities in penehyclidine hydrochloride injection

A penehyclidine hydrochloride and a detection method are applied in the directions of measuring devices, instruments, scientific instruments, etc., and can solve the problems that the requirements of strict control of drug impurities cannot be met, the detection results can only be semi-quantitative, and the detection sensitivity is low. Achieve the effect of good accuracy, improved detection sensitivity, and high sensitivity

Active Publication Date: 2014-12-24
CHONGQING XIANYANG PHARMA TECH CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

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 injection
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  • Method of detecting impurities in penehyclidine hydrochloride injection

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Main instruments and chromatographic conditions:

[0045] TRACE GC MLTRA gas chromatograph, equipped with hydrogen flame ionization detector (FID), temperature 300°C, automatic sampler, Chromeleon chromatography workstation.

[0046] Chromatographic column: Rtx?-5 Amine (30m×0.25mm, 0.5μm)

[0047] Column temperature: the initial temperature is 90°C, keep for 1 minute, raise the temperature to 300°C at a rate of 8°C per minute, and keep for 8 minutes;

[0048] [0026] Column flow rate: 2. 5ml / min;

[0049] Inlet temperature: 190°C;

[0050] Split ratio: 4:1;

[0051] Injection volume: 2 μl.

[0052] Penehyclidine hydrochloride injection was provided by Chongqing Xianyang Pharmaceutical Technology Co., Ltd., specification 1ml:1mg, batch number 110900.

[0053] The impurity II reference substance was provided by Chongqing Xianyang Pharmaceutical Technology Co., Ltd., batch number 110601.

[0054] The impurity III reference substance was purchased from Sigma, batch...

Embodiment 2

[0061] Embodiment 2: Methodological verification test

[0062] According to the chromatographic conditions and operating methods of Example 1, the specificity, precision, linearity, detection limit and quantification limit, sample addition recovery rate and stability of the method were respectively verified by methodology, and the results were as follows:

[0063] (1) Specificity:

[0064] 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 1.365min, 2.558min, 2.935min, and 3.326min, the retention time of impurity II is 5.121min, the retention time of impurity III is 5.543min, and the retention time of penehyclidine is 14.945min, indicating that the solv...

Embodiment 3

[0099] With reference to the method of Example 1, change the kind of dissolved reference substance acid solution, the results are shown in Table 6:

[0100] Table 6 The results of the investigation of the acid type and concentration of the dissolved reference substance

[0101]

[0102] The results showed that the impurities Ⅱ and Ⅲ were well separated by treating the reference substance with various dilute acids, and satisfactory results could be obtained. The product is the hydrochloride salt, so dilute hydrochloric acid is preferred.

[0103]

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Abstract

The invention discloses a method of detecting two impurities containing a quinuclidine ring in a penehyclidine hydrochloride injection. 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 injection is subjected to vacuum rotary evaporation to remove the solvent in the injection, 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 salified by adding an acid firstly, then is processed as the same processing manner for the sample solution to be detected, and is 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 injection, 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 injection. Background technique [0002] Penehyclidine hydrochloride injection, the main component is penehyclidine hydrochloride, chemical name: 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine hydrochloride. The chemical formula is: [0003] [0004] I [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...

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 CHONGQING XIANYANG PHARMA TECH CO LTD
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