Method for simultaneously preparing high-purity podophyllotoxin and deoxidized podophyllotoxin from sabina vulgaris

A technology of deoxypodophyllotoxin and podophyllotoxin, which is applied in the direction of organic chemistry, etc., to achieve the effects of simple operation, high separation efficiency and expansion of column capacity

Inactive Publication Date: 2015-01-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This technology allows for efficient isolating and separating highly pure materials from plant material that contains both glucosylceroline (GC) and phytolitholedicta (PE). These two molecules have unique structures but they may differ due to their chemical composition or physical characteristics such as size, shape, surface charge, etc., making them difficult to separate effectively without expensive equipment like liquid extraction techniques. By utilizing this technique, researches on these products could lead to better understanding how chemistry works together during various stages of production processes.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the quality and quantity of bergenisks found throughout North America through isolative distillations involving specific types of chantercytotaxes called cathaytestropes. These bergensys contain three main bioactive agents - phytate esters, α-,β-,γ-,δ-(Liu et al., 2004); they play important roles in nutritional support systems like nuts and vegetables. However, these materials cannot be separated effectively without expensive methods like columnchromatography which requires significant capital assets and operating expenses.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In the working drum of the main engine of the countercurrent chromatography in this embodiment, the column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube is 2.5 liters. The solvent system adopts carbon tetrachloride: ethyl acetate: methanol: water = 17:6:15:3.5 (volume ratio).

[0032] Take 3.4L of carbon tetrachloride, 1.2L of ethyl acetate, 3.0L of methanol, and 0.7L of water, and mix them thoroughly in a 10L mixing kettle. After standing for stratification, separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pressed into the working drum of the main engine by air pressure. Take by weighing 20 grams of the ethanol extraction extract of Juniper juniper, dissolve with 200mL of the lower phase solution, filter to obtain the ethanol extraction extract solution of Juniper juniper for dissolving, and set aside. Open the countercurrent chromatographic separation device, adjust the ...

Embodiment 2

[0034] In the working drum of the main engine of the countercurrent chromatography in this embodiment, the column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube is 2.5 liters. The solvent system adopts carbon tetrachloride: ethyl acetate: methanol: 0.10 mol / L acetic acid aqueous solution = 17:6:15:3.5 (volume ratio).

[0035] Take 3.4 L of carbon tetrachloride, 1.2 L of ethyl acetate, 3.0 L of methanol, and 0.7 L of 0.10 mol / L aqueous acetic acid solution, mix them thoroughly in a 10 L mixing kettle, and separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pressed into the working drum of the main engine by air pressure. Take by weighing 20 grams of the ethanol extraction extract of Juniper juniper, dissolve with 200mL of the lower phase solution, filter to obtain the ethanol extraction extract solution of Juniper juniper for dissolving, and set aside. Open the countercurrent chromato...

Embodiment 3

[0037]The column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube in the main machine working drum of the countercurrent chromatography in this embodiment is about 1.2 liters. The solvent system adopts carbon tetrachloride: ethyl acetate: methanol: water = 19:6:16:3 (volume ratio).

[0038] Take 1.9L of carbon tetrachloride, 0.6L of ethyl acetate, 1.6L of methanol, and 0.3L of water, and mix them thoroughly in a 5L mixing kettle. After standing for stratification, separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pressed into the working drum of the main engine by air pressure. Take by weighing 10 grams of the ethanol extraction extract of Juniper juniper, dissolve with 100mL of the lower phase solution, filter to obtain the ethanol extraction extract solution of Juniper juniper for dissolving, and set aside. Open the countercurrent chromatographic separation device, adjust the main ...

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Abstract

The invention discloses a method for simultaneously preparing high-purity podophyllotoxin and deoxidized podophyllotoxin from sabina vulgaris. The method takes a high-speed counter-current chromatography device as separating and purifying equipment and comprises the following steps of: preparing a solvent system which forms an immobile phase and a mobile phase, and pressing and suffusing the prepared immobile phase into a working drum of a main machine in an air pressure mode to rotate the main machine, wherein an upper phase is the immobile phase and a lower phase is the mobile phase; then pumping dissolved ethanol extraction extract of sabina vulgaris and the mobile phase at a preset flow rate, and respectively collecting and podophyllotoxin and deoxidized podophyllotoxin components (obtained through separation) from the mobile phase according to a detection spectrogram. The liquid-liquid partition chromatography separation and preparation method disclosed by the invention completely overcomes the defects of irreversible adsorption, contamination, denaturation and the like of a sample on a solid filler and is simple and convenient to operate, low in organic solvent consumption and high in separation efficiency; and the purity of the obtained product is higher than 98%.

Description

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Claims

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Application Information

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Owner ZHEJIANG UNIV
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