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Separation and purification method of salidroside in natural rhodiola sachalinensis

A technology for separation and purification of salidroside, which is applied in the field of separation and purification of salidroside in natural rhodiola, can solve the problems of complex operation of adsorption and desorption processes, high requirements for process technical conditions, unstable product quality and the like , to achieve the effect of facilitating continuous production, good separation effect, and improving the utilization rate of raw materials

Inactive Publication Date: 2013-04-03
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Column chromatography can obtain relatively high-purity salidroside, but the loss of active ingredients is serious, and the yield is too low, so it is only suitable for the preparation of trace standards; during the use of ultrafiltration purification ultrafiltration membranes, membrane fouling is easy to cause The flux of the membrane drops sharply, and a large amount of alkali and acid are used in the membrane cleaning process, and the separation selectivity is poor, and the product quality is unstable; while the ethanol precipitation method removes impurities, the obtained dry extract has a high viscosity and is easy to absorb moisture , which brings inconvenience to the later process operation. This method consumes a lot of alcohol, has high cost, and takes a long time to process. The macroporous resin adsorption method has stricter requirements for the pretreatment of the treatment liquid, higher requirements for the process and technical conditions, and the operation of the adsorption and desorption process. More complex, lower product concentration, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 Preparation of an aqueous solution of the active ingredient of Rhodiola rosea in the present invention.

[0027] Take an appropriate amount of Tibetan rhodiola raw material and slice it, the thickness of which is about 0.2 cm; then extract the slices in an aqueous solution at a temperature of 65°C with ultrasonic waves for 60 minutes, filter to remove solid slices and particles to obtain a reddish-brown extract; cool down to 20°C , after adjusting the pH to 9.5 with 0.1 mol / liter sodium hydroxide aqueous solution, add 95% ethanol solution of 3 times the volume of the extract, that is, the volume ratio of water extract to 95% ethanol is 1:3, cool down to 5°C and stand still for 24 Hours; after separating the flocculent precipitate, the supernatant is concentrated under reduced pressure at a vacuum degree of about 0.08MPa and a temperature of 50°C until no ethanol is distilled off to obtain a brown-red aqueous solution rich in active ingredients of Rhodiol...

Embodiment 2

[0028] Example 2 The separation and purification method of salidroside in natural Rhodiola rosea in the present invention.

[0029] Take an appropriate amount of Rhodiola rosea raw materials and slice them, the thickness of which is about 0.5 cm; then extract the slices in an aqueous solution at a temperature of 70°C with ultrasonic waves for 40 minutes, filter and remove solid slices and particles to obtain a reddish-brown extract; cool down to 20°C , after adjusting the pH to 10.5 with 0.1 mol / liter sodium hydroxide aqueous solution, add 95% ethanol solution with 5 times the volume of the extract, that is, the volume ratio of water extract to 95% ethanol is 1:5, cool down to 10°C and stand still for 24 Hours; after separating the flocculent precipitate, the supernatant was concentrated under reduced pressure at a vacuum degree of about 0.08MPa and a temperature of 60°C until no ethanol was distilled off to obtain an aqueous solution rich in Rhodiola rosea active ingre...

Embodiment 3

[0031] Example 3 The separation and purification method of salidroside in natural Rhodiola rosea in the present invention.

[0032] Take an appropriate amount of Tibetan Rhodiola rosea raw material and slice it, the thickness of which is about 0.4 cm; then extract the slice with ultrasonic waves in an aqueous solution at a temperature of 75°C for 30 minutes, and filter to obtain the extract; after cooling down to room temperature, oxidize it with 0.1 mol / L hydrogen After adjusting the pH of the sodium aqueous solution to 11, add 95% ethanol solution of 4 times the volume of the extract, that is, the volume ratio of the water extract to 95% ethanol is 1:4, cool down to 5°C and stand still for 24 hours; separate the supernatant Under the conditions of vacuum degree of about 0.08MPa and temperature of 55°C, the water extract 3 was obtained by concentrating under reduced pressure until no ethanol was distilled off.

[0033] Take Rhodiola rosea water extract 3 and n-hexanol solv...

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Abstract

The invention relates to a separation and purification method of salidroside in natural rhodiola sachalinensis. The separation and purification method is characterized by comprising the steps of: slicing the natural rhodiola sachalinensis serving as a raw material; carrying out ultrasonic water leaching, low-temperature alcohol participation and vacuum concentration to obtain a water extract; carrying out solvent stripping and impurity removal, solvent extracting and back-extracting to obtain a high-purity salidroside water solution; and finally, carrying out vacuum concentration, absolute ethyl alcohol crystallization, separation and drying to obtain the salidroside. The purity of the salidroside extracted by adopting the separation and purification method can reach above 97 percent; the yield in a purification stage of a novel process is greatly increased, the yield in an extraction and purification stage of salidroside can reach above 70 percent, and the raw material utilization rate is increased; an addition product tyrosol enriching solution can be obtained; and the separation and purification method is simple in process, convenient for operation and suitable for industrialized massive production.

Description

technical field [0001] The invention belongs to the technical field of natural product separation technology, and in particular relates to a method for separation and purification of salidroside in natural rhodiola rosea. Background technique [0002] Rhodiola belongs to the genus Rhodiola of Crassulaceae, a perennial herb or subshrub. It is distributed in my country's Tibet, Yunnan, Guizhou, Northeast, Gansu, Xinjiang, Sichuan and other regions. It contains salidroside, flavonoids, Amino acid, tyrosol, trace elements, coumarin and more than 40 kinds of compounds have remarkable effects in anti-hypoxia, anti-fatigue, anti-virus, enhancement of body immunity, anti-aging, anti-radiation, and two-way regulation of body functions. Among them, salidroside is the main pharmacological active ingredient of Rhodiola rosea plant, which has wide demand and application value in pharmaceuticals, cosmetics and health food industries. [0003] The extraction and separation metho...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 申淑锋
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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