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Detection method for determining impurities in penehyclidine hydrochloride through high performance liquid chromatography (HPLC)

A penehyclidine hydrochloride and a detection method are applied in the directions of measuring devices, instruments, scientific instruments, etc., and can solve the problems of inability to meet impurity detection requirements, large operation errors, and inconspicuous color development, and achieve high accuracy and improved Detection sensitivity, the effect of high sensitivity

Active Publication Date: 2015-01-21
重庆科塞亚医药科技有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thin-layer chromatography has the disadvantages of being more affected by the environment such as temperature, humidity, reagent type, sample application technology, etc., poor reproducibility, low sensitivity, poor reproducibility, and inconspicuous color development. At the same time, the detection results can only be semi-quantitative. And the operation error is large
In view of the fact that the quality requirements of medicines are getting higher and higher, and the impurity control is becoming increasingly strict, this standard can no longer meet the requirements of impurity detection.

Method used

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  • Detection method for determining impurities in penehyclidine hydrochloride through high performance liquid chromatography (HPLC)
  • Detection method for determining impurities in penehyclidine hydrochloride through high performance liquid chromatography (HPLC)
  • Detection method for determining impurities in penehyclidine hydrochloride through high performance liquid chromatography (HPLC)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1 The selection of wavelength

[0044] Take the appropriate amount of impurity A, impurity B, and penhyclidine hydrochloride respectively, dissolve them in methanol, and carry out ultraviolet full-wavelength scanning in the wavelength range of 190-400nm. The results show that: penehyclidine hydrochloride, impurity A, and impurity B There is a large absorption in the range of ~220nm. Among them, impurity A has maximum absorption at 208nm, impurity B has maximum absorption at 209nm, and penhyclidine hydrochloride has maximum absorption at 208nm. Since the cut-off wavelength of acetonitrile is 190nm, in order to ensure the separation and detection of impurities as much as possible and to avoid the interference of low-band, 210nm±10nm was selected as the detection wavelength.

[0045]

Embodiment 2

[0046] The determination of embodiment 2 sample

[0047] Main chromatographic conditions:

[0048] Mobile phase: mobile phase A: acetonitrile; mobile phase B: 0.02mol / L potassium dihydrogen phosphate (containing 0.5% triethylamine, dilute phosphoric acid to adjust pH=3.0). Carry out gradient elution according to the table below:

[0049]

[0050] Flow rate: 1.0ml / min.

[0051] Column temperature: 35°C.

[0052] Detection wavelength: 210nm.

[0053] Injection volume: 20μl

[0054]Preparation of the test solution: Accurately weigh 10 mg of penhyclidine hydrochloride for the test, add solvent (mobile phase A: mobile phase B=32:68) to dissolve and set the volume to 10 ml, and obtain the test solution (1 mg / ml).

[0055] Preparation of the reference substance solution: Accurately weigh 10 mg of the impurity reference substance, add solvent (mobile phase A: mobile phase B=32:68) to dissolve and set the volume to 100ml, precisely pipette 1ml, add solvent to dissolve and set...

Embodiment 3

[0058] Example 3 Methodology Verification Test

[0059] According to the chromatographic conditions of Example 2, methodological verification was carried out from aspects of specificity, precision, linearity, detection limit and quantification limit, stability, and the results are as follows:

[0060] (1) Specificity:

[0061] Take the solvent, the test solution (pentehyclidine hydrochloride solution), the mixed solution of impurity A and B reference substance, the mixed solution of penehyclidine hydrochloride and impurity reference substance A and B, and inject samples in sequence. The test results showed that the peak eluting time of the solvent was between 2min and 5min, the retention time of penhyclidine hydrochloride was 11.633min and 12.420min, the retention time of impurity A was 42.035min, and the retention time of impurity B was 25.577min. The results showed that the separation between the solvent and the reference substance solution was good, and there was n...

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Abstract

The invention discloses a detection method for determining two impurities in penehyclidine hydrochloride. In the method, high performance liquid chromatography (HPLC) is employed. Acetonitrile and 20 mmol / L monopotassium phosphate (containing 0.5% of triethylamine with the pH being adjusted to 3.0 through diluted phosphoric acid) are employed as a mobile phase. The contents of the impurities are determined through gradient elute. During determination, a solvent is prepared according to an initial mobile phase proportion, namely, the acetonitrile : the 20 mmol / L monopotassium phosphate (containing 0.5% of triethylamine with the pH being adjusted to 3.0 through diluted phosphoric acid) is 32:68. The penehyclidine hydrochloride is prepared into a sample solution through the solvent and an impurity referent substance solution is prepared through the same method to obtain the impurity referent substance solution. The sample solution, the impurity referent substance solution are injected directly. A chromatogram is collected and the contents of the impurities are calculated according to an external standard method according to the areas of peaks. The method is simple in operation, is high in sensitivity, can be used in quantitative determination, is high in accuracy and is good in reproducibility so that product quality of the penehyclidine hydrochloride can be effectively controlled and clinical medication is ensured to be safe and effective.

Description

technical field [0001] The invention relates to a detection method for impurities in medicines, in particular to 3[2-cyclopentyl-2-phenyl-2(2-cyclopentyl-2-hydroxyl-2-phenylethoxy) in penhyclidine hydrochloride ) Detection method of ethoxy]quinuclidane hydrochloride, α-phenyl-α-cyclopentyl-α-hydroxyethanol. [0002] Background technique [0003] Penehyclidine hydrochloride, chemical name: 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy)quinuclidine hydrochloride. The 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 b...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/36
Inventor 姚有良蒋艇刘晓燕
Owner 重庆科塞亚医药科技有限责任公司
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