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Preparation method of cocaine hydrochloride standard substance

A standard substance, cocaine technology, applied in the preparation of test samples, etc., can solve the problems of cocaine hydrochloride standard substance containing many impurities, large production process differences, unstable product quality, etc., to achieve good product performance stability, The preparation time is short and the effect is suitable for popularization and application

Inactive Publication Date: 2012-10-31
公安部禁毒情报技术中心 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the deficiencies in the prior art that the standard substance of cocaine hydrochloride contains more impurities, the preparation and production process of the standard substance is greatly different, the product quality is unstable, the preparation speed is slow, the reagents used are expensive, the process is complicated, and the recovery rate is low. , provide a preparation method with fast preparation speed, high recovery rate and high-purity cocaine hydrochloride standard substance

Method used

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  • Preparation method of cocaine hydrochloride standard substance
  • Preparation method of cocaine hydrochloride standard substance
  • Preparation method of cocaine hydrochloride standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] refer to figure 1 , follow the steps below:

[0032] a. Weigh 6 g of cocaine hydrochloride sample, add 15 ml of methanol to dissolve, and then add 15 ml of absolute ethanol to it to adjust the polarity of the solution to make it soluble in flow.

[0033] b. The sample solution obtained in step a is injected into the medium-pressure preparation system for preparation and purification. The chromatographic conditions are: 20-45 μm HILIC chromatographic column, and the filler is a mixed filler with a mass ratio of secondary amine and tertiary amine of 3:2, using 80g+80g+ 80g three branches are set in series, flow rate 30ml / min, detection wavelength 234nm, auxiliary wavelength 280nm, mobile phase: A is chromatographic pure hexane, B is chromatographic pure absolute ethanol, gradient elution, gradient conditions are as follows:

[0034] Time (min) Start B% End B%

[0035] 40 60 100

[0036] 20 100 100

[0037] c. The receiving solution at 12-44min, i.e. the main peak re...

Embodiment 2

[0044] a. Prepare a cocaine hydrochloride sample solution with a concentration of 0.6g / ml in methanol, and add ethanol to adjust the polarity of the solution according to the ratio of the sample to ethanol being 0.6g:1.6ml;

[0045] b. The sample solution obtained in step a is prepared and purified by a medium pressure preparation system. The chromatographic conditions are: the packing of the chromatographic column is amino-bonded silica gel packing, the detection wavelength is 234 nm, the auxiliary wavelength is 280 nm, and the mobile phase: A is chromatographically pure hexane, and B is Chromatographic pure absolute ethanol, gradient elution;

[0046] c. The prepared main peak receiving solution was concentrated under reduced pressure in a rotary evaporator at 45° C. to obtain a crude cocaine product, and the crude cocaine product was prepared with methanol with a concentration of 0.35g / ml. The ratio of the sample to ethanol was 0.35g Add ethanol in a ratio of 1.6 ml to a...

Embodiment 3

[0053] Prepare a cocaine hydrochloride sample solution with a concentration of 0.6g / ml in methanol, and add ethanol to adjust the polarity of the solution according to the ratio of the sample to ethanol being 0.6g:1.2ml;

[0054] b. The sample solution obtained in step a is prepared and purified by a medium pressure preparation system. The chromatographic conditions are: the packing of the chromatographic column is amino-bonded silica gel packing, the detection wavelength is 234 nm, the auxiliary wavelength is 280 nm, and the mobile phase: A is chromatographically pure hexane, and B is Chromatographic pure absolute ethanol, gradient elution;

[0055] c. The prepared main peak receiving solution was concentrated under reduced pressure in a rotary evaporator at 40° C. to obtain a crude cocaine product. This crude cocaine product was prepared with methanol with a concentration of 0.35g / ml. The ratio of the sample to ethanol was 0.35g Add ethanol in a ratio of 1.4 ml to adjust t...

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Abstract

The invention belongs to a preparation method of a standard substance, and in particular relates to a preparation method of a cocaine hydrochloride standard substance. The invention solves the problems that in the prior art, the cocaine hydrochloride standard substance is high in impurity content, the preparation process of the standard substance is large in difference, the quality of the product is unstable, the preparation speed is low, the process is complex and the recovery rate is low, and provides a cocaine hydrochloride standard substance preparation method which is high in preparation speed and recovery rate and can obtain high-purity cocaine hydrochloride standard substances. The preparation method comprises the following steps of: preparing a cocaine hydrochloride sample solution and regulating the solution polarity; preparing and purifying the obtained sample solution by a medium-pressure preparation system; concentrating main-peak reception liquid obtained by preparing at reduced pressure to obtain a crude product of cocaine; preparing the crude product of cocaine into a solution, regulating the solution polarity, and purifying the obtained solution again; and concentrating the main-peak reception liquid obtained by preparing at reduced pressure to obtain the cocaine hydrochloride standard substance. The preparation method is simple in process and high in recovery rate, and is suitable for popularization and application.

Description

technical field [0001] The present invention relates to a method for preparing a standard substance, more specifically, a method for preparing a standard substance of cocaine hydrochloride. Background technique [0002] Cocaine, also known as cocaine, is the first natural alkaloid (C 17 H 21 NO 4 ), a long-acting ester local anesthetic, with high fat solubility, strong penetrating power, good affinity for nerve tissue, and good surface anesthetic effect. Its vasoconstrictive effect may be related to blocking the reuptake of norepinephrine by nerve endings. It is highly toxic. Small doses can excite the cerebral cortex and produce euphoria. As the dose increases, the respiratory, vascular movement and vomiting centers are excited. In severe cases, convulsions may occur; Central respiratory depression occurs, and heart failure is caused by myocardial depression. Cocaine is absorbed from the site of application (mucosal and gastrointestinal tract), metabolized by esterase ...

Claims

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Application Information

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IPC IPC(8): G01N1/38G01N1/34G01N1/40
Inventor 冯超白燕平王洪宇刘伟李运华刘建波汪群杰
Owner 公安部禁毒情报技术中心
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