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Method for preparing rosmarinic acid chemical reference substances from three kinds of alpine sage plants

A technology of sage and aromatic acid chemistry, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large loss, no literature report, cumbersome process, etc., and achieve high recovery rate , low price, simple process effect

Inactive Publication Date: 2016-06-15
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no report on the preparation of phenolic acid compounds from Alpine Salvia plants. Chinese patent (CN1995007) reports that extraction, addition of antioxidants or adjustment of pH to acidity and then filtration, the filtrate is passed through polyamide resin, ion exchange Resin or macroporous resin column chromatography is used to separate, then adjust the pH to acidic, stand still, crystallize, and filter to produce rosmarinic acid with a purity of about 90%. The process is cumbersome and the loss is large. , but there is no literature report on the preparation of rapid acquisition of large-scale rosmarinic acid from Ganxi sage, sticky sage and Kangding sage

Method used

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  • Method for preparing rosmarinic acid chemical reference substances from three kinds of alpine sage plants
  • Method for preparing rosmarinic acid chemical reference substances from three kinds of alpine sage plants
  • Method for preparing rosmarinic acid chemical reference substances from three kinds of alpine sage plants

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Effect test

Embodiment 1

[0025] Embodiment 1 prepares the method for rosmarinic acid chemical reference substance from three kinds of alpine sage plants, comprising the following steps:

[0026] ⑴Microporous resin (MCI) impurity removal:

[0027] 200.0g of the brownish-red extract-like alcoholic extract of Salvia villosa produced by a conventional method is dissolved in an ethanol solution with a volume fraction 10% of its mass 10 times, and is filtered to obtain filtrate A, and the filtrate A is placed on a microporous resin column For separation, first remove impurities by eluting with 5 times column volume of aqueous solution, then carry out step gradient elution with 5 times column volume, 30% methanol solution and 80% methanol solution, and collect 30% methanol water eluate. The methanol water eluate was dried under reduced pressure at a vacuum degree of 0.06 MPa and a temperature of 70° C. to obtain 36.4 g of crude phenolic acid components.

[0028] in:

[0029] The ratio of the ethanol extrac...

Embodiment 2

[0039] Embodiment 2 prepares the method for rosmarinic acid chemical reference substance from three kinds of alpine sage plants, comprising the following steps:

[0040] ⑴Microporous resin (MCI) impurity removal:

[0041] 100.0g of the reddish-brown extract-like alcoholic extract of Salvia ganxie prepared by a conventional method is dissolved in an ethanol solution with a volume fraction 30% of 5 times of its mass, and is filtered to obtain filtrate A, and the microporous resin column on the filtrate A is For separation, first remove impurities by eluting with 2 times column volume of aqueous solution, then use 2 times column volume, 50% methanol solution and 60% methanol solution to carry out step gradient elution, and collect 50% methanol water eluate, the The methanol water eluate was dried under reduced pressure at a vacuum degree of 0.09 MPa and a temperature of 50° C. to obtain 17.6 g of crude phenolic acid components.

[0042] in:

[0043] The ratio of the alcohol ext...

Embodiment 3

[0053] Embodiment 3 prepares the method for rosmarinic acid chemical reference substance from three kinds of alpine sage plants, comprising the following steps:

[0054] ⑴Microporous resin (MCI) impurity removal:

[0055] 500.0g of the brownish-red extract-like Sage Kangding ethanol extract prepared by a conventional method is dissolved in an ethanol solution with a volume fraction 20% of 8 times its mass, and is filtered to obtain filtrate A, which is separated by a microporous resin column , first eluted with 3 times column volume of aqueous solution to remove impurities, then carried out step gradient elution with 3 times column volume, methanol solution with a volume fraction of 40%, and 70% methanol solution, and collected 40% methanol water eluate, the methanol The water eluate was dried under reduced pressure at a vacuum degree of 0.08 MPa and a temperature of 60° C. to obtain 86.2 g of crude phenolic acid components.

[0056] in:

[0057] The ratio of Kangding sage a...

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Abstract

The invention relates to a method for preparing a rosmarinic acid chemical reference substance from three types of high mountain salvias. The method comprises the following steps: (1) performing pore resin decontamination: dissolving an alcohol extract of one of salvia roborowskii, salvia przewalskii and salvia prattii with ethanol solution, filtering, separating on a pore resin column, eluting with water solution for decontaminating, then performing stepwise gradient elution with methanol solution, collecting 30% to 50% of methyl alcohol water eluate, and drying the methyl alcohol water eluate under reduced pressure to obtain a phenolic acid type component crude product; (2) performing silica gel column enrichment: performing silica gel column chromatography separation on the phenolic acid type component crude product, then eluting, and collecting a fraction with an Rf value of 0.18 to 0.22; drying the fraction under reduced pressure to obtain a faint yellow and powdery rosmarinic acid crude product; (3) performing preparative liquid chromatography purification: dissolving the rosmarinic acid crude product with methanol solution, filtering, performing preparative liquid chromatography separation, collecting a chromatography peak fraction, and drying the chromatography peak fraction under reduced pressure to obtain the white and powdery reference substance. The method is simple in process and easy for large scale.

Description

technical field [0001] The invention relates to a method for preparing a chemical reference substance of rosmarinic acid, in particular to a method for preparing a chemical reference substance of rosmarinic acid from three kinds of alpine sage plants. Background technique [0002] Salvia L. is the largest genus of Lamiaceae. There are three main species of sage on the Qinghai-Tibet Plateau, Salvia Roborowskii, Salvia przewalskii Maxim. and Salvia Kangding. (Salvia prattii). Modern studies have shown that the chemical constituents in sage plants mainly include phenolic acids and terpenes. At present, there are no quality control index ingredients for the three Alpine Salvia plants, Ganxi Sage, Clary Sage and Kangding Sage. Rosmarinic acid is the content of these three Salvia plants. Higher phenolic acid compounds, due to the high polarity of the compound and severe tailing on silica gel thin-layer chromatography, it is difficult to obtain high-purity rosmarinic acid referen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/56
CPCC07C67/56C07C69/732
Inventor 党军邵赟张莉王启兰梅丽娟陶燕铎苑祥岳会兰
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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