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Method of preparing high-purity polyprenol lipid by means of both high-speed countercurrent chromatography and high performance liquid chromatography

A technology of high-speed countercurrent chromatography and high-performance liquid chromatography, applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., to achieve the effect of long time, high extraction rate and few steps

Active Publication Date: 2013-06-12
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are currently no articles or patents reporting the separation of polyprenol by high-speed countercurrent chromatography

Method used

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  • Method of preparing high-purity polyprenol lipid by means of both high-speed countercurrent chromatography and high performance liquid chromatography
  • Method of preparing high-purity polyprenol lipid by means of both high-speed countercurrent chromatography and high performance liquid chromatography
  • Method of preparing high-purity polyprenol lipid by means of both high-speed countercurrent chromatography and high performance liquid chromatography

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Experimental program
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Embodiment 1

[0031] Embodiment 1 high-speed countercurrent chromatography standard sample separation

[0032] 1. Experimental equipment:

[0033] FastChrome analytical high-speed countercurrent chromatography (Jiangyin Countercurrent Technology Co., Ltd.); separation column volume: 25mL; value range: 0.56 to 0.91; OptiChromeA semi-preparative high-speed countercurrent chromatography (Jiangyin Countercurrent Technology Co., Ltd.); spiral tube separation column (revolution Radius: 80cm; value range: 0.50~0.80; spiral tube inner diameter: 1.59mm), single column volume 180mL, double column volume 360mL.

[0034] 2. Experimental materials:

[0035] Analysis of pure isomer phenolic samples catechol, resorcinol, hydroquinone; n-hexane, ethyl acetate, methanol, distilled water

[0036] 3. Preparation of solvents and samples:

[0037] Prepare methanol mixed solution of phenolic samples, mixed sample concentration: catechol 20mg / mL + resorcinol 20mg / mL + hydroquinone 10mg / mL; use 80% methanol sol...

Embodiment 2

[0058] Embodiment 2 high-speed countercurrent chromatography and high-performance liquid chromatography combined method

[0059] The first step, polyprenol lipid extraction

[0060] Dry fresh plant leaves rich in polyprenyl alcohol lipids, dry in the shade at room temperature, crush to powder below 100 mesh, add anhydrous acetone or any solvent in C1-C3 alcohol, preferably anhydrous acetone or ethanol, the leaf powder is not mixed with The mass ratio of the solvent is 1:8~30, preferably 1:8~15, soaking at room temperature~80°C for 10~72 hours, such as 25~50°C, static soaking for 30~50 hours; or microwave extraction or ultrasonic extraction for 10 hours ~ 60 minutes, extraction power 100W ~ 1000W, twice, combined extracts, vacuum recovery organic solvent, concentrate is polyprenol lipid ointment, ointment relative to plant leaf powder yield 4 ~ 10%, polyprenol Lipid content 5-20%;

[0061] The second step, high-speed countercurrent chromatographic separation

[0062] (1) Sel...

Embodiment 3

[0070] Example 3 High-speed countercurrent chromatography polyprenol separation experiment

[0071] 1. Solvent preparation: n-Hexane: Acetonitrile: Acetone = 3:1:1 Prepare 2000 mL by volume ratio, the upper phase is the stationary phase, and the lower phase is the mobile phase.

[0072] 2. Sample preparation: Take 50 mg of the polyprenyl alcohol lipid ointment in Example 1 and dissolve it in 50 mL of mobile phase.

[0073] 3. System balance: pump the stationary phase at a speed of 50mL / min, pump the mobile phase at a speed of 5mL / min, and start

[0074] 4. OptiChrome TM A-300 is centrifuged forward, observe that the output of UV3000 reaches the system balance, and calculate the stationary phase retention rate: 60%

[0075] 5. Sample loading: inject the sample into OptiChrome through the sample loading valve TM A-300 in. Forward centrifugation: OptiChrome TM A-300 is set to positive centrifugal rotation, setting.

[0076] 6. Reverse centrifugation: set the separation flow r...

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Abstract

The invention discloses a method of preparing high-purity polyprenol lipid by means of both a high-speed countercurrent chromatography and a high performance liquid chromatography. Ginkgo leaves, pine needles and mulberry leaves are used as raw materials, alcohol of anhydrous acetone or anhydrous carbon 1 - carbon 3 is used as extraction solvent, and extraction is carried out through low temperature microwaves or ultrasonic waves to prepare polyprenol paste. Solvents, such as normal hexane, acetonitrile and acetone, are proportionally mixed to form a high-speed countercurrent solvent system, the high-speed countercurrent solvent system is kept still after sufficiently mixed, an upper phase is a fixed phase, a low phase is a flowing phase, the polyprenol paste is dissolved in the lower phase to serve as a product to be tested, the fixed phase is filled in a separation column of a high-speed countercurrent chromatographic instrument, the rotation speed is set as 500-1000 rounds / min, the fixed phase flows to the flowing phase with the flowing speed 1-5mL / min and is detected in an ultraviolet detecting device with wavelength 210-230mm, in the centrifuge process, normal phase centrifugal rotation is adopted for 180-240min at first, then opposite phase centrifugal rotation is adopted for 30-60 min, when the flowing phase starts to flow out of a chromatographic column, distillate is collected, different constituents are collected in a classified mode, and after high performance liquid chromatography (HPLC) detection, the polyprenol lipid with the purity 60-90% is prepared.

Description

1. Technical field [0001] The invention relates to a method for extracting and separating polyprenyl alcohol lipid compounds from plant leaves by using high-speed countercurrent chromatography combined with high-performance liquid chromatography, and belongs to the field of natural drug separation and medical and health care product applications. 2. Background technology [0002] At present, most of the separation technologies for natural products in the world use supercritical extraction technology, macroporous resin column chromatography technology, molecular distillation technology, membrane separation technology, etc., but for natural products with very low content and high biological activity, facing social challenges Progress and mankind's requirements for refined products with high-tech content are extremely lacking in new technologies that can not only achieve the separation and purification of high-purity substances, but also achieve considerable preparation capabili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/76C07C33/02C08F116/04
Inventor 王成章闵凡芹何源峰原姣姣陈虹霞叶建中周昊
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY