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
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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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