Method for removing procymidone in ginsenoside through macroreticular resin adsorption-supercritical CO2 elution

A ginsenoside and resin adsorption technology, applied in pharmaceutical formulations, medical preparations containing active ingredients, plant raw materials, etc., can solve the problems of explosion-proof equipment, extremely high operation requirements, loss of ginsenosides, etc., to shorten the production cycle, reduce The effect of high production cost and saponin recovery rate

Inactive Publication Date: 2015-12-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] For the removal of pesticide residues in ginseng, the publication number is CN1723969, and the Chinese invention patent on January 25, 2006 discloses a "supercritical CO 2 Method for Removing Organochlorine Pesticides from Ginseng, using supercritical CO 2 Solvent, ethanol are the method for entraining agent to remove the pesticide residue in ginseng, although have certain effect but be difficult to make organochlorine content drop below 0.1ppm, and because entraining agent is ethanol, ginsenoside is easily soluble in ethanol, can cause Massive loss of ginsenosides
In addition, the publication number is CN101156881, and the Chinese invention patent application published on April 9, 2008 discloses "A Method for Removing Pesticide Residues in Ginseng", which uses propane as a solvent to remove organic chlorine residual pesticides in ginseng. The method of purification and removal, although the removal effect of pesticide residues is remarkable, but propane is a flammable and explosive gas, which has extremely high requirements for equipment explosion-proof and operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, using D-101-1 type macroporous adsorption resin to adsorb and combine supercritical CO 2 To elute and remove procymidone in ginsenosides, the steps are as follows:

[0020] Step 1. Pretreatment of D-101-1 macroporous adsorption resin: Fill D-101-1 macroporous adsorption resin to the height of 2 / 3 of the adsorption column, add ethanol to the adsorption column to make the liquid level Above the level of the macroporous adsorption resin, soak for 24 hours; then use ethanol to pass through at a flow rate of 2BV / h, wash until there is no fat-soluble impurities in the outflowing ethanol, and then wash with distilled water until there is no peculiar smell; then use 4% NaOH Soak for 12 hours, wash with distilled water until neutral; finally soak with 5% HCl for 12 hours, wash with distilled water until neutral; wet-pack the treated D-101-1 macroporous adsorption resin into a column;

[0021] Step 2. Preparation of ginsenoside sample solution: Weigh 2.5 g of ginse...

Embodiment 2

[0026] Embodiment 2: Adopt AB-8 type macroporous adsorption resin to adsorb in conjunction with supercritical CO 2 To elute and remove procymidone in ginsenosides, the steps are as follows:

[0027] Step 1. Weigh a certain amount of AB-8 macroporous adsorption resin, treat it according to Step 1 of Example 1, and finally pack the treated resin into a column by wet method.

[0028] Step 2. Preparation of ginsenoside sample solution: Weigh 5 g of ginsenoside and add 100 mL of distilled water to prepare a ginsenoside sample solution with a solid-to-liquid ratio of 0.05 g / mL.

[0029] Step 3, resin adsorption: measure the ginsenoside sample solution 1 times the volume of the AB-8 type macroporous adsorption resin, and use a peristaltic pump to pass through the adsorption column at a flow rate of 2BV / h.

[0030] Step 4, resin drying: dry the AB-8 macroporous adsorption resin adsorbed with the ginsenoside sample solution in an oven at 45° C. for 4 hours;

[0031] Step 5, supercrit...

Embodiment 3

[0033] Embodiment 3: Adopt H-103 type macroporous adsorption resin to adsorb in conjunction with supercritical CO 2 To elute and remove procymidone in ginsenosides, the steps are as follows:

[0034] Step 1. Weigh a certain amount of H-103 macroporous adsorption resin, process it according to Step 1 of Example 1, and finally pack the processed resin into a column by wet method.

[0035]Step 2, prepare ginsenoside sample solution, same as Example 2.

[0036] Step 3, resin adsorption: same as Example 2.

[0037] Step 4, resin drying: drying the H-103 macroporous adsorption resin adsorbed with the ginsenoside sample solution in an oven at 50° C. for 4 hours;

[0038] Step 5, supercritical elution: put the dried H-103 macroporous adsorption resin into a supercritical extraction column, and then proceed sequentially, the first step of procymidone removal: supercritical CO 2 The pressure is 20MPa, the temperature is 45°C, the entrainer flow rate is 1mL / min, the entrainer is compo...

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PUM

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Abstract

The invention discloses a method for removing procymidone in ginsenoside through macroreticular resin adsorption and supercritical CO2 elution. The method comprises the following steps: pretreating macroreticular resin; preparing a ginsenoside sample solution; adsorbing the ginsenoside sample solution with the resin, and drying; carrying out supercritical elution, namely, packing the dried macroreticular resin into a supercritical extraction column, then carrying out removal of procymidone and elution of ginsenoside, and drying the sample to obtain the ginsenoside product with the content of procymidone less than 10ppb. With the adoption of the method, the removal rate of procymidone is 96.7% or above, and the recovery rate of ginsenoside is 89% or above; in addition, while removal of procymidone and elution of ginsenoside are carried out, the regeneration of the resin is realized, the production cost is reduced, and the production cycle is shortened.

Description

technical field [0001] The invention belongs to the technical field of removal of residual chemical components in plant extracts, in particular to a macroporous adsorption resin adsorption-supercritical CO 2 A method for removing procymidone in ginsenosides in combination with elution, Background technique [0002] Ginsenosides have the functions of enhancing the body's immunity, anti-fatigue, relieving toxins, and inducing apoptosis of cancer cells. Long-term use can prolong life. However, due to the long growth cycle of ginseng, pesticide residues accumulate in ginseng through soil and other environmental factors, resulting in the enrichment of pesticide residues in ginseng (hereinafter referred to as pesticide residues). Higher levels of pesticide residues. Excessive pesticide residue content has largely become the main limiting factor for the export of ginseng and ginseng products in my country. At the same time, eating products with excessive pesticide residues is als...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/258
Inventor 唐韶坤李广涛
Owner TIANJIN UNIV
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