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Preparation method for high purity rhynchophylline

A high-purity technology for rhynchophylline, which is applied in the field of preparation of high-purity rhynchophylline, can solve the problems of poor thermal stability of rhynchophylline, easy decomposition, and low yield of rhynchophylline, etc., and achieves short preparation period and high production volume. Large, the effect of reducing the loss of samples

Inactive Publication Date: 2012-01-11
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods all have certain adsorption to the product, and the heat stability of rhynchophylline is relatively poor, promptly has partial decomposition at 80 ℃, and its ester bond is easily decomposed by heating, and is easily converted into isorhynchophylline under polar conditions, The conversion rate is above 60%, resulting in extremely low yield of rhynchophylline

Method used

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  • Preparation method for high purity rhynchophylline

Examples

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Effect test

Embodiment 1

[0018] Uncaria medicinal material is crushed to 20 meshes, 10kg is taken, 4 times the amount of 5% sodium carbonate solution is added for ultrasonic extraction for 1 hour, the liquid is filtered off, and then 5 times the amount of dichloromethane is added for ultrasonic extraction 3 times, the dichloromethane extract is used to recover the reagent and concentrated to 100ml. Take chloroform, methanol, and water, mix and layer them in a separatory funnel at a ratio of 6:7:3, take the upper phase and adjust the pH to 7.5 with triethylamine, make it a stationary phase, inject it into a high-speed countercurrent chromatography column, and make it full , turn on the host, rotate at 700rpm, pump into the lower phase, after dynamic balance, adjust the flow rate to 2ml / min, and inject the concentrated solution from the injection valve at the same time, the ultraviolet detector will monitor online, collect the target components, refrigerate and crystallize, filter out and dry, 980 mg of...

Embodiment 2

[0021] Uncaria medicinal material is crushed to 20 meshes, 10kg is taken, and 5 times the amount of 5% sodium carbonate solution is added for ultrasonic extraction for 1 hour, the liquid is filtered off, and then 7 times the amount of dichloromethane is added for ultrasonic extraction twice, and the dichloromethane extract is used to recover reagents and concentrated to 150ml. Take chloroform, methanol, and water, mix and layer them in a separating funnel at a ratio of 8:5:3, take the upper phase and adjust the pH to 8 with triethylamine, make it a stationary phase, inject it into a high-speed countercurrent chromatography column, make it full, and turn it on The main engine rotates at 1000rpm, and pumps into the lower phase. After dynamic balance, the flow rate is adjusted to 4ml / min. At the same time, the concentrated solution is injected from the injection valve, and the ultraviolet detector is monitored online. The target components are collected, refrigerated and crystalli...

Embodiment 3

[0024] Uncaria medicinal material is crushed to 20 meshes, 10kg is taken, 4 times the amount of 5% sodium carbonate solution is added for ultrasonic extraction for 1 hour, the liquid is filtered off, and then 5 times the amount of dichloromethane is added for ultrasonic extraction 3 times, the dichloromethane extract is used to recover the reagent and concentrated to 100ml. Take n-hexane, ethyl acetate, methanol, and water in a ratio of 3:5:2:6, mix and layer in a separatory funnel, remove the phase and adjust the pH to 7.5 with triethylamine, make it a stationary phase, and inject it into a high-speed countercurrent In the chromatographic column, make it full, turn on the host, rotate at 800rpm, pump into the upper phase, after dynamic equilibrium, adjust the flow rate to 1ml / min, and inject the concentrated solution from the injection valve at the same time, and the ultraviolet detector will monitor online to collect the target components. Refrigerate and crystallize, filter...

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Abstract

The present invention provides a preparation method for high purity rhynchophylline. The method comprises: crushing rhynchophylline medicinal material to have a particle size of 20-60 meshes; adding the crushed rhynchophylline to a sodium carbonate solution, wherein the amount of the sodium carbonate solution is 4-5 times the amount of the crushed rhynchophylline, and the sodium carbonate content in the sodium carbonate solution is 5%; carrying out ultrasonic extraction for 1 hour, and removing liquid through filtering; adding dichloromethane to carry out ultrasonic extraction for 2-3 times, recovering the regent from the extracting solution; concentrating the extracting solution to small volume; carrying out separation through high speed countercurrent chromatography, carrying out online monitoring through an ultraviolet detector; collecting the target component; carrying out cold preservation and crystallization to obtain the high purity rhynchophylline. With the method provided by the present invention, the separation treatment is performed through the high speed countercurrent chromatography; the production period is short; the product yield is high; the product purity is more than 95%.

Description

technical field [0001] The invention relates to a method for preparing high-purity rhynchophylline, in particular to a method for preparing high-purity rhynchophylline by high-speed countercurrent chromatography. [0002] Background technique [0003] Rhynchophylline is an indole alkaloid, chemical name Corynixan-16-carboxylic acid, 16, 17-didehydro-17-methoxy-2-oxo-, methyl ester, (7B, 16E, 20a)-, molecular formula C 22 h 28 N 2 o 4 , molecular weight 384.46, CAS No. 76-66-4, molecular structure: [0004] [0005] Rhynchophylline is an alkaloid in Uncaria uncariae of the Rubiaceae plant. Rhynchophylline can inhibit peripheral vasoconstriction, reduce vascular resistance, lower blood pressure, and have anti-platelet aggregation and anti-thrombotic effects, with low toxicity and few side effects. [0006] The existing methods for extracting high-purity rhynchophylline generally use packed column chromatography, such as silica gel, alumina and reverse silica gel. For...

Claims

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Application Information

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IPC IPC(8): C07D471/20
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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