Method for testing tropine alcohol of residual intermediate product in synthesizing Troipisetron

A technique for detecting tropisetron and a detection method, which is applied in the detection field of tropinol, can solve problems such as no absorption peak of tropinol, failure to reach the limit of residual amount, and inability to control the residual amount, etc. Simple, high-sensitivity effect

Active Publication Date: 2006-02-01
QINGDAO PURUISEN MEDICINE SCI & TECH CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

However, in the actual synthetic production process of preparing tropisetron, tropine alcohol has no ultraviolet absorption, and when using high-performance liquid phase to detect tropisetron, tropine alcohol does not show an absorption peak, and its residual amount cannot be controlled
Using an evaporative light scattering detector, the precision is not enough to meet the requirements for detecting the residual amount limit
And the detection of residual intermediate tropinol in the synthesis of tropisetron sensitively and rapidly, after searching, there is no literature report at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of the test solution: take an appropriate amount of tropisetron, add methanol to dissolve and quantitatively dilute to make a 25mg / ml solution; accurately weigh an appropriate amount of pure tropinol, add methanol to dissolve and quantitatively dilute to make a 0.05mg / ml solution Reference substance solution: respectively take 15 microliters of the above-mentioned need testing solution and reference substance solution on the same silica gel G thin-layer plate, mix acetone:ammonia water at a volume ratio of 80:20 to make a developing agent, and develop in a chromatographic cylinder , take it out, and dry it; spray the bismuth potassium iodide solution evenly on the thin layer with a sprayer, and dry it; then spray the sodium nitrite solution (now prepared) evenly on the thin layer with a sprayer, and dry it; Sprayer sprays the bismuth potassium iodide solution evenly on the thin layer, and blows dry; Wherein, the spray distance of the sprayer and the thin laye...

Embodiment 2

[0028] Take an appropriate amount of tropisetron, add methanol to dissolve and quantitatively dilute to make a 25mg / ml test solution; accurately weigh an appropriate amount of pure tropinol, add methanol to dissolve and quantitatively dilute to make a 0.05mg / ml reference solution; Take 15 microliters of the above-mentioned test solution and reference solution respectively on the same silica gel G thin-layer plate, mix acetone:ammonia water at a volume ratio of 99:1 to make a developing agent, develop in a chromatography cylinder, take it out, and let it dry in the air. Dry; Spray bismuth potassium iodide solution evenly on the thin layer with a sprayer, and blow dry; then spray sodium nitrite solution (now prepared) evenly on the thin layer with a sprayer, and dry; The bismuth potassium solution is evenly sprayed on the thin layer and blown dry; wherein, the spray distance between the sprayer and the thin layer is 0.4 meters; the preparation method of the bismuth potassium iodi...

Embodiment 3

[0030] Take an appropriate amount of tropisetron, add methanol to dissolve and quantitatively dilute to make a 25mg / ml test solution; accurately weigh an appropriate amount of pure tropinol, add methanol to dissolve and quantitatively dilute to make a 0.05mg / ml reference solution; Take 15 microliters of the above-mentioned test solution and reference solution respectively on the same silica gel G thin-layer plate, mix acetone:ammonia water at a volume ratio of 90:10 to make a developing agent, develop in a chromatography cylinder, take it out, and let it dry in the air. Dry; Spray bismuth potassium iodide solution evenly on the thin layer with a sprayer, and blow dry; then spray sodium nitrite solution (now prepared) evenly on the thin layer with a sprayer, and dry; The bismuth potassium solution is evenly sprayed on the thin layer and dried; wherein, the spray distance between the sprayer and the thin layer is 0.8 meters; the preparation method of the bismuth potassium iodide ...

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Abstract

A method for detecting residual intermediate of tropaic alcohol in tropisetron synthesis includes preparing test solution and control solution , dropping them separately on the same silica gel G thin layer plate , using acetone ¿C ammonia water as developing agent to carry out thin layer chromatography determination, developing chromatographic cylinder, using developer of bismuth potassium iodide solution with assistance of sodium nitride solution to develop color and checking colour developed result.

Description

technical field [0001] The invention relates to a detection method for tropinol, in particular to a detection method for residual intermediate tropinol in the synthesis of tropisetron. Background technique [0002] Tropisetron is a potent and selective 5-HT3 receptor antagonist developed by Novartis and launched in the UK in 1992 under the trade name Navoban. It is used for the prevention and treatment of nausea and vomiting caused by radiotherapy and chemotherapy. At present, the drug has been marketed in dozens of countries around the world, and its indications have been expanded to prevent and treat nausea and vomiting during radiotherapy and chemotherapy in children, and prevent and treat postoperative nausea and vomiting in adults. [0003] Because of its definite curative effect, tropisetron has been widely used in large and medium-sized hospitals. Facing nearly 600,000 cancer patients undergoing radiotherapy and chemotherapy every year in the country, its market pros...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/90G01N30/94
Inventor 贡肖巍徐文芳郑家晴张建礼翟海民王丽崔美兰
Owner QINGDAO PURUISEN MEDICINE SCI & TECH CO LTD
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