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A kind of detection method of impurity in penehyclidine

The technology of penehyclidine and its detection method is applied in the field of detection of impurities in penehyclidine, which can solve the problems of failing to meet the limit requirements of drug impurities, unreported detection, large operating errors, etc., achieving good accuracy and improving The effect of high detection sensitivity and accuracy

Active Publication Date: 2016-06-01
CHONGQING XIANYANG PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The national standard WS1-(X-026)-2004Z adopts TLC to detect impurity Ⅲ, but the TLC detection is often affected by the environment such as temperature, humidity, reagent type, sampling technique, etc. It has the disadvantages of low sensitivity and inconspicuous color rendering. At the same time, the detection 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 limit requirements for strict control of drug impurities.
The detection of impurity IV and impurity VI has not been reported

Method used

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  • A kind of detection method of impurity in penehyclidine
  • A kind of detection method of impurity in penehyclidine
  • A kind of detection method of impurity in penehyclidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Main instruments and chromatographic conditions:

[0048] Main main instruments and chromatographic conditions:

[0049] TRACEGCULTRA gas chromatograph, equipped with hydrogen flame ionization detector (FID), temperature 300°C, automatic sampler, Chromeleon chromatography workstation.

[0050] Chromatographic column: Rtx?-5Amine (30m×0.25mm, 0.5μm)

[0051] 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.

[0052] Column flow rate: 2.5ml / min;

[0053] Inlet temperature: 190°C;

[0054] Split ratio: 4:1;

[0055] Injection volume: 2ul.

[0056] Penehyclidine was provided by Chongqing Xianyang Pharmaceutical Technology Co., Ltd., batch number 110900.

[0057] The impurity II reference substance was provided by Chongqing Xianyang Pharmaceutical Technology Co., Ltd., batch number 110601.

[0058] Impurity III was purchased from Sigma, lot number MKBF3377V.

[0...

Embodiment 2

[0067] Embodiment 2: Methodological verification test

[0068] According to the chromatographic conditions and operating methods of Example 1, methodological verification was carried out from the aspects of specificity, precision, linearity, detection limit and quantitation limit, sample recovery rate, and stability, and the results are as follows:

[0069] (1) Specificity:

[0070] Take the solvent DMF, the test solution (pentehyclidine solution), the reference substance solution, and the mixed solution of penehyclidine and the reference substance II, III, IV, V, and VI, respectively, and inject samples in sequence. The results show that the solvent has peaks with retention times of 1.370min, 2.565min, 2.939min, and 3.331min, and the retention times of impurities II, III, IV, V, and VI are 5.128min, 5.552min, 9.765min, 9.912min, and 11.420min, respectively. min, the retention time of penehyclidine is 14.948min. The separation between the solvent and penehyclidine and the im...

Embodiment 3

[0107] With reference to the method of Example 1, the temperature of the injection port is investigated. The results are shown in Table 5:

[0108] Table 5 Injection port temperature inspection results (%)

[0109]

[0110] The above results show that when the temperature of the injection port is measured within the range of 150-230°C, the impurities II, III, IV, V, and VI are well separated and accurate determination can be realized.

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Abstract

The invention discloses a method of detecting five impurities comprising 3-quinuclidone, 3-quinuclidinol, phenylcyclopentyl ketone, phenyl cyclopentyl ethylene oxide, and alpha-benzyl-alpha-cyclopentyl-alpha hydroxy ethanol in penehyclidine. The method adopts a gas chromatographic method to detect contents of the impurities. During detection, the penehyclidine is dissolved with dimethylformamide 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 and guarantees safety and effectiveness of clinical medication.

Description

technical field [0001] The invention relates to a detection method for impurities in medicines, in particular to 3-quinine, 3-quinine alcohol, phenylcyclopentyl ketone, phenylcyclopentyl oxirane, α- Method for the detection of phenyl-alpha-cyclopentyl-alpha-hydroxyethanol. Background technique [0002] Penhyclidine, chemical name: 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine. Chemical formula is [0003] [0004] I [0005] The hydrochloride of this product 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 姚有良李凤君刘晓燕
Owner CHONGQING XIANYANG PHARMA TECH CO LTD
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