Method of removing procymidone residue in ginseng and American ginseng extracts by resin method

A resin, pore adsorption technology, used in chemical instruments and methods, alkali metal compounds, alkali metal oxides/hydroxides, etc.

Inactive Publication Date: 2014-05-07
INST OF SPECIAL ANIMAL & PLANT SCI OF CAAS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention discloses a method for removing procymidone residues in ginseng and American ginseng extracts by resin method, which solves the problem of removing pesticide residues by solvent extraction Secondary pollution, poor safety and other related issues

Method used

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  • Method of removing procymidone residue in ginseng and American ginseng extracts by resin method
  • Method of removing procymidone residue in ginseng and American ginseng extracts by resin method

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Add 1500mL of purified water into a 3000ml reactor equipped with a thermometer, condensing reflux device and stirring, add 15g of gelatin while stirring, raise the temperature to 60°C, after the gelatin is completely dissolved, add 50g of styrene, 450g of Divinylbenzene, 100g toluene, 100g dichloroethane, the mixture of 2.5g benzoyl peroxide, etc. After the organic mixture forms uniform droplets of a certain size in the dispersion medium solution, the temperature is raised to 76 ° C, and the reaction is carried out for 5 hours. The temperature was raised to 80° C. to cure for 9 hours to stop the reaction. Rinse with a large amount of water, sieve, control the particle size between 20-70 mesh, and dry to obtain macroporous polystyrene resin white balls. Take 100g of white balls, add 600g of dichloroethane, swell at room temperature for 2 hours, add the catalyst anhydrous aluminum trichloride (3.33g / 30min) in 3 times, and raise the temperature to 80°C for 10h. Cool down,...

Embodiment 2

[0044]Add 1500mL of purified water into a 3000ml reactor equipped with a thermometer, condensing reflux device and stirring, add 15g of gelatin while stirring, raise the temperature to 60°C, after the gelatin is completely dissolved, add fully mixed 150g of styrene, 350g The mixture composed of divinylbenzene, 200g toluene, 2.5g benzoyl peroxide, etc. After the organic mixture forms uniform droplets of a certain size in the dispersion medium solution, heat up to 76°C, react for 5 hours, heat up to 80°C and solidify for 9 hours, the reaction stopped. Rinse with a large amount of water, sieve, control the particle size between 20-70 mesh, and dry to obtain macroporous polystyrene resin white balls. Take 100g of white balls, add 600g of dichloroethane, swell at room temperature for 2 hours, add catalyst anhydrous ferric chloride (6.67g / 30min) in 3 times, raise the temperature to 80°C for 10h. Cool down, extract dichloroethane, wash with water, put it into a Soxhlet extractor, ex...

Embodiment 3

[0048] Precisely weigh the LKS11 resin (Example 1) and place it in a suitable container, soak it in 95% ethanol for 24 h, and wash it with distilled water until it has no alcohol smell. After washing away the alcohol smell, soak in 10% NaOH solution for more than 3 hours, then wash with distilled water until neutral; finally soak in 10% HCl solution for more than 3 hours, wash with distilled water until neutral, and wet-pack the pretreated resin in column. Accurately weigh 20.00 g of ginseng extract, add 200 mL of distilled water, stir and let it stand for 2 h, then fully mix to prepare a 0.1 g / mL sample solution. Pipette 2 times the volume of the resin sample solution into the resin column, absorb for more than 1 h, and control the flow rate of 2-5 mL / min to pass through the column. First wash with distilled water of 1 times the volume of the resin, then elute with 50% ethanol of 6 times the volume of the resin, and collect the eluate. The evaporation equipment is sealed to...

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Abstract

The invention provides a method of removing procymidone residue in ginseng and American ginseng extracts by a resin method, and meanwhile provides hypercross-linked macroporous resin adaptive to the method and a preparation process. Synthetic LKS-11 resin is combined with the molecular structure of procymidone, macroporous resin with unique microcellular structure distribution is synthesized in a targeted manner, and the macroporous resin is quoted to the removal technology of the pesticide procymidone. Procymidone can be effectively removed by extracts which take different parts of ginseng and American ginseng as raw materials. The method has the advantages of simple and convenient operation, convenience in recycle disposal of resin, low production and operation cost and good safety, the recovery rate of products reaches up to over 92%, the removal effect is good, and the removal rate of residual procymidone is over 90%.

Description

technical field [0001] The present invention provides a resin method for removing procymidone residues in ginseng and American ginseng extracts, and simultaneously provides an ultra-high cross-linked macroporous adsorption resin suitable for the above method and a preparation process, which belongs to the category of residual chemical components in plant extracts Remove technical fields. Background technique [0002] Ginseng ( panax ginseng C.A.Mey.) and American ginseng ( Panax quinquefolius L.) is a perennial herbaceous plant of Araliaceae, both of which are precious Chinese herbal medicines, not only the raw materials of Chinese herbal medicines and Chinese patent medicines, but also prepared by pretreatment, extraction, concentration, separation or purification, drying, packaging and other processes The extract is also an emerging modern traditional Chinese medicine product, which is used in medical care, beauty and skin care, food and beverage and other fields, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/36C08F212/08C08F2/20C08F4/34C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 崔丽丽郑培和毛剑英高博刘玉甫王英平
Owner INST OF SPECIAL ANIMAL & PLANT SCI OF CAAS
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