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Detection method for alpha-tropine as impurity in hydrochloric acid tropisetron

A technology of tropisetron hydrochloride and detection method, which is applied to measurement devices, instruments, scientific instruments and other directions, can solve the problems of large operation error, low reproducibility, low detector sensitivity, etc., and achieves improved detection sensitivity and reliable inspection. Basics, the effect of increasing controllability

Active Publication Date: 2012-07-11
SHANDONG QIDU PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, α-tropine itself has no ultraviolet absorption, and it is difficult to analyze it with a high-performance liquid chromatography ultraviolet detector. When using an evaporative light detector and a differential refractive index detector, the limit detection of α-tropine cannot be realized. Detector sensitivity is low
In the European Pharmacopoeia (EP7.0), thin-layer chromatography is used to detect impurity A (α-tropine alcohol) in tropisetron hydrochloride, but the presence of impurity A (α-tropine alcohol) in the detection of thin-layer chromatography is affected by temperature, humidity, reagent type, point However, it has the disadvantages of more environmental impact and low reproducibility, such as sampling technology, and at the same time, the detection results can only be semi-quantitative, and the operation error is large.
Relevant sensitive and quantitative detection method for α-tropine alcohol in tropisetron hydrochloride has not been reported in the literature at home and abroad after retrieval

Method used

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  • Detection method for alpha-tropine as impurity in hydrochloric acid tropisetron
  • Detection method for alpha-tropine as impurity in hydrochloric acid tropisetron
  • Detection method for alpha-tropine as impurity in hydrochloric acid tropisetron

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Experimental program
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Effect test

Embodiment 1

[0071] Preparation of the test solution: take an appropriate amount of tropisetron hydrochloride, accurately weighed, first dissolve with a little water, then dilute with acetone and make a 30mg / ml solution at constant volume, as the test solution; take α-Tropisetron An appropriate amount of Pinol reference substance was accurately weighed, dissolved and diluted with acetone to make a 0.06 mg / ml solution as the reference substance solution; the above-mentioned solvent, the test solution and the reference substance solution were taken respectively for headspace injection according to the law, and the chromatograms were collected (Such as figure 1 , 2 , 3), calculate the result by the surface method based on the peak area.

[0072] Chromatographic conditions:

[0073] Injection port: split flow, temperature 260°C;

[0074] Chromatographic column: polyethylene glycol as stationary phase or similar in polarity Recommended: HP-INNOWAX 0.32mm×0.25μm×30m;

[0075] Column tempera...

Embodiment 2

[0083] Preparation of the test solution: take an appropriate amount of tropisetron hydrochloride, accurately weighed, first dissolve with a little water, then dilute with acetone and make a 30mg / ml solution at constant volume, as the test solution; take α-Tropisetron An appropriate amount of Pinol reference substance was accurately weighed, dissolved with acetone and diluted to make a 0.06 mg / ml solution as the reference substance solution; the above-mentioned test solution and the reference substance solution were respectively taken for headspace sampling according to the law, and the chromatograms were collected (contrast product solution such as Figure 4 ), the results were calculated by the surface method based on the peak area.

[0084] Chromatographic conditions:

[0085] Injection port: split flow, temperature 250°C;

[0086] Chromatographic column: polyethylene glycol as stationary phase or similar in polarity Recommended: HP-INNOWAX 0.32mm×0.25μm×30m;

[0087] Co...

Embodiment 3

[0095] Preparation of the test solution: take an appropriate amount of tropisetron hydrochloride, accurately weighed, first dissolve with a little water, then dilute with acetone and make a solution of 20 mg / ml at constant volume, as the test solution; take α-Tropisetron An appropriate amount of pin alcohol reference substance, accurately weighed, dissolved with acetone and diluted to make a 0.04mg / ml solution, as a reference substance solution; respectively take the above-mentioned test solution and reference substance solution according to headspace injection, and collect chromatograms (α -tropine alcohol reference substance solution such as Figure 5 ), the results were calculated by the surface method based on the peak area.

[0096] Chromatographic conditions:

[0097] Injection port: split flow, temperature 260°C;

[0098] Chromatographic column: polyethylene glycol as stationary phase or similar in polarity Recommended: HP-INNOWAX 0.32mm×0.25μm×30m;

[0099] Column ...

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Abstract

The invention relates to a detection method for alpha-tropine as impurity in hydrochloric acid tropisetron, which is characterized by adopting the gas chromatography for detection, and particularly includes the following steps: (1) preparing sample hydrochloric acid tropisetron solution with concentration of 10mg / m1 to 30mg / ml; (2) preparing reference sample alpha-tropine solution with the concentration of 0.02mg / m1 to 0.06mg / m1; (3) performing headspace sample injection and chromatogram acquisition; and (4) calculating the result through the appearance method based on the peak area. The invention has the characteristics that the detection method is convenient, quantitative and sensitive, and can be widely applied to the control and improvement of the medicine quality.

Description

technical field [0001] The invention relates to a method for detecting alpha-tropine, in particular to a method for detecting alpha-tropine in tropisetron hydrochloride. Background technique [0002] Tropisetron hydrochloride, chemical name: 3-indolecarboxylic acid (8-methyl-8-azabicyclo[3.2.1]-3α-octyl) ester hydrochloride. Chemical formula is [0003] [0004] It is used to prevent and treat nausea and vomiting reactions caused by tumor chemotherapy and radiotherapy. It is a peripheral neuron and central nervous system 5-hydroxytryptamine 3 (5-HT 3 ) receptors are potent and highly selective competitive antagonists. Certain substances, including some chemotherapeutic drugs, stimulate the release of serotonin from chromaffin-like cells in the visceral mucosa, which induces the gag reflex with nausea. This product is mainly by selectively blocking the presynaptic 5-HT of peripheral neurons 3 receptors to inhibit the vomiting reflex, in addition, its antiemetic effect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 郑家晴黄国英张建礼刘绪贵
Owner SHANDONG QIDU PHARMA
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