Process for synthesizing and detecting scopolamine derivates

Abstract

The invention provides a synthesis method and a detection method for scopolamine derivatives. The synthesis method comprises the following steps that: under the existence of carbonate, bicarbonate or other alkaline matter, quaternization reaction is carried out to scopolamine and halogenated hydrocarbon or halogen olefin; dehydration treatment is carried out to reactants and solvent before the reaction; when the reaction begins, the alkaline matter which is two times the molar weight of the scopolamine is added; when the reaction is carried out for four hours, the alkaline matter is filtered out, and filtrate continues to react; the solvent is selected from any one or mixture of ethanol, methanol and acetonitrile. The detection method comprises the following steps that: the content of scopolamine derivatives is determined through high performance liquid chromatography; a mobile phase preparation method is to mix methanol or acetonitrile with ammonium salt buffer solution according to the proportion of 20-50:80-50; the ammonium salt buffer solution respectively uses formic acid, glacial acetic acid or phosphoric acid to regulate ammonium formate, ammonium acetate or ammonium dihydrogen phosphate with the pH value less then 4; flow rate is between 0.5 and 2.0 ml / min; the absorption is detected at a position with the wavelength between 210 and 250 nanometers.

Description

technical field [0001] The invention provides a method for synthesizing and detecting scopolamine and its derivatives. The invention belongs to the field of medicine preparation technology and detection means. Background technique [0002] Scopolamine, chemical name 6β, 7β-epoxy-1αH, 5αH-tropane-3α-ol (-) tropinate, is an anticholinergic drug with a high affinity to M-choline receptors. The clinical routes of administration include transdermal, nasal cavity, and oral administration, but because M-choline receptors are widely distributed in the central and peripheral areas, scopolamine has high lipophilicity, so no matter which route of administration is adopted, scopolamine can easily pass through the blood. The brain barrier has a strong effect on the central system, and the drug has large toxic and side effects, the dosage is difficult to control, and the safety of use is low. In recent years, people have been trying to modify the structure of scopolamine to obtain compo...

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Problems solved by technology

Moreover, as the reaction time prolongs, the by-products increase, and it is difficult to separate the by-products at the end of the reaction.

When detecting the content of the final product, non-aqueous titration methods with large errors and low accuracy are often used. Even if the high-performance liquid chromatography with high accuracy is used for detection, sodium heptanesulfonate, sodium octanesulfonate or sodium octanesulfonate must be added to the mobile phase. Sodium hexanesulfonate and other expensive ion-pairing reagents, and such structurally modified compounds have no characteristic absorption peaks in the ultraviolet region, so the detection wavelength used is not greater than 210nm, but there is terminal absorption at this wavelength, which affects the results. accuracy

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