CN103772578A - Method of removing procymidone residue in ginseng and American ginseng extracts by resin method - Google Patents
Method of removing procymidone residue in ginseng and American ginseng extracts by resin method Download PDFInfo
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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
The invention provides a kind of resin method and remove the residual method of procymidone in ginseng, Radix Panacis Quinquefolii extract, the superhigh cross-linking macroporous adsorbent resin and the preparation technology that are applicable to aforesaid method are provided simultaneously, have belonged to the removal technical field of residual chemical composition in plant milk extract.
Background technology
Ginseng (
panax ginsengc.A.Mey.) and Radix Panacis Quinquefolii (
panax quinquefoliusl.) be Araliaceae perennial root herbaceous plant, the two is rare traditional Chinese medicine, be not only the raw material of the prepared slices of Chinese crude drugs and Chinese patent medicine, the extract making through technological processs such as pre-treatment, extraction, concentrated, isolated or purified, dry, packings, also be the emerging former medicine product of modern Chinese herbal medicine, be applied to the fields such as health care, beauty and skin care, food-drink, there is objective economic benefit and social benefit.
Chemical pesticide is widespread use because it has the features such as, wide adaptability efficient, quick-acting, easy to operate to harmful organism and remarkable in economical benefits, becomes the requisite important measures of most of disease controls, causes in ginseng and soil residual.Remains of pesticide people's body accumulation to a certain amount of the human body vitals such as immunity system, neural system and reproductive system, Digestive tract that directly jeopardize human body are brought out light to cough, muscle numbness, heavy to the disease such as diabetes and cancer.In recent years, food safety affair occurs time and again, pesticide residue cause that food, drug quality safety problem also become World Focusing problem, and therefore removing ginseng and Radix Ginseng extract Pesticide Residues is also the important topic that we face, and has very important realistic meaning.
Chinese patent 201310105162.7 discloses take normal hexane, ethyl acetate and acetone as extraction agent, the method that Radix Ginseng extract Pesticides procymidone is removed, this method has certain effect to removing procymidone residual quantity, but because the extraction agent using is virose organic reagent, very easily cause the secondary pollution of Radix Ginseng extract, security is poor.Normal hexane can enter human body by the approach such as respiratory tract, skin, and Long Term Contact can cause human body to occur the chronic poisoning symptoms such as headache, dizzy, weak, numbness of the limbs, and serious causing fallen in a swoon, unconsciousness, even death.Ethyl acetate has hormesis to eye, nose, throat, and high density sucks can cause the anesthetic action of carrying out property, causes acute lung edema, and liver, renal impairment continue a large amount of suction, can cause respiratory paralysis.Acetone is mainly inhibition, the anesthetic action to central nervous system, and the infringement of liver, kidney and pancreas may appear in high density contact to one or two people.Use normal hexane, ethyl acetate and acetone, as extraction solvent, production unit stopping property and operation are had to higher requirement,, there is harm to operator's health in the easy contaminate environment of the medium-term and long-term use of production process simultaneously.
Therefore, need one sample not to be caused to secondary pollution, safety and environmental protection, the de-procymidone method that production run cost is low and the high removal effect of product recovery rate is good.
summary of the invention
The associated problem such as the present invention discloses a kind of resin method and removes the residual method of procymidone in ginseng, Radix Panacis Quinquefolii extract, has solved the secondary pollution to extract of the existence of solvent extration removal pesticide residue, and security is poor.
The present invention also further provides a kind of superhigh cross-linking macroporous adsorbent resin and preparation technology, be applicable to remove ginseng and Radix Panacis Quinquefolii extract, cauline leaf, fruit and the residual method of total saponins Pesticides procymidone, for realizing ginseng, the residual removal object of Radix Panacis Quinquefolii extract procymidone.
Technical solution of the present invention is as follows:
In conjunction with molecular weight and the molecular structure feature of procymidone, take styrenic as monomer, take multi-vinyl monomer as linking agent, the condition low suspension polymerization existing at pore-creating agent obtains macroporous polystyrene Archon, gained Archon carries out Friedel-Crafts alkylated reaction under swelling agent exists take Lewis acid as catalyzer, gained resin is novel macroporous adsorbent resin LKS11, this resin has unique microvoid structure and distributes, and the procymidone in ginseng and Radix Panacis Quinquefolii extract is had to good removal effect.Utilize the selective adsorption of macroporous adsorbent resin, the sample of the resin column of flowing through is had to MIN absorption, and sample Pesticides procymidone is had to absorption to greatest extent.Use this physical method safe, product itself is not produced to secondary pollution; Technology novelty, production run cost is low, removal effect good, product recovery rate is high.
Technical problem to be solved by this invention be synthetic a kind of microvoid structure distribute unique macroporous adsorbent resin, to utilize resin method to remove in ginseng, Radix Panacis Quinquefolii procymidone residual.
A kind of superhigh cross-linking macroporous adsorbent resin provided by the present invention, is the macroporous adsorbent resin LKS11 that it is unique that a kind of microvoid structure distributes, and its structural formula is as follows:
(wherein, n=1,2,3 ...)
the preparation method of macroporous adsorbent resin LKS11 of the present invention, comprises the steps:
1) macroporous polystyrene Archon preparation
Take by weight styrene monomer 10-30, linking agent 70-90, pore-creating agent 50-150, polymerization starter 0.5-1.5, said components is placed in to dispersion medium together, under 60-100 ℃ of condition, react suspension polymerization in 12-20 hour and obtain macroporous polystyrene Archon;
2) crosslinking reaction after
Step (1) gained macroporous polystyrene Archon is joined in swelling agent, under room temperature swelling 2 hours, add catalyzer Lewis acid, at 70-120 ℃, carry out Friedel-Crafts alkylated reaction, reaction times is 8-16 hour, obtains macroporous adsorbent resin, called after LKS11 resin.
the preparation method of superhigh cross-linking macroporous adsorbent resin of the present invention, is characterized in that:
Step 2) temperature of reaction is 80-100 ℃, the reaction times is 10-14 hour.
the preparation method of superhigh cross-linking macroporous adsorbent resin of the present invention, is characterized in that:
Styrene monomer described in step 1) is selected from the one in vinylbenzene, vinyl toluene, alpha-methyl styrene, ethyl styrene, optimization styrene;
Described linking agent is selected from multi-vinyl monomer, as divinylbenzene, methacrylate ethylene glycol, trimethylolpropane trimethacrylate, and preferably divinylbenzene;
Described pore-creating agent is selected from aromatic hydrocarbons as toluene, dimethylbenzene; Higher alcohols is as butanols, hexanol, and alkanes is as normal heptane, ethylene dichloride, 200
#gasoline, whiteruss, solid paraffin, ester class is as butylacetate, ethyl acetate, preferably toluene and gasoline, pore-creating agent can use separately or any two to three kinds mix and use, aromatic hydrocarbons is classified 2:1-1:2 as with the ratio of alkanes;
Described polymerization starter is selected from organo-peroxide, as peroxidation paraphenylene terephthalamide, peroxide-2-ethyl hexanoic acid tert-butyl, peroxidation-2 ethyl hexanoic acid tert-pentyl ester etc., and preferably peroxidation paraphenylene terephthalamide;
Described dispersion agent is selected from gelatin or polyvinyl alcohol or Natvosol, and consumption is the 0.5%-2% of dispersion medium weight;
Step 2) described Lewis acid is selected from Zinc Chloride Anhydrous, aluminum trichloride (anhydrous), FERRIC CHLORIDE ANHYDROUS or anhydrous stannic chloride, and the consumption of catalyzer is the 10%-40% of macroporous polystyrene Archon total amount;
Described swelling agent is selected from ethylene dichloride or oil of mirbane, and consumption is 4-8 times of macroporous polystyrene Archon weight.
a kind of resin method provided by the invention is removed the residual method of procymidone in ginseng, Radix Panacis Quinquefolii extract, comprises the following steps:
1) resin pre-treatment: LKS11 resin prepared by claim 2 is first used after 30%～95% alcohol immersion 24 h, is washed till without alcohol taste with distilled water; After washing most alcohol taste, use 1%-10% NaOH solution soaking 3 ~ 5 hours, be then washed till neutrality with distilled water; Finally use 1%-10% HCl solution soaking 3 ~ 5 hours, distilled water is washed till neutrality;
2) dress post: resin wet method good pre-treatment is loaded in post;
3) sample solution preparation: take pending sample water-soluble, leave standstill and it was fully dissolved in 2 ~ 5 hours after stirring, be made into the sample solution that concentration is 0.05～0.1 g/mL;
4), absorption: the sample solution that pipettes 1～10 times of resin volume is added in resin column, adsorbs 1 ~ 2 hour, and coutroi velocity 2～5 mL/min cross post;
5), desorb: first wash with the distilled water of 1～4 times of resin volume, then use 30%～95% ethanol elution of 1～10 times of resin volume, collect elutriant;
6) reclaim reagent;
7) dry: the sample aqueous solution after recovery solvent carries out drying treatment and obtains the residual product of low procymidone.
positively effect of the present invention is:the molecular structure of synthetic LKS-11 resin-bonded procymidone, synthesize targetedly and there is the macroporous adsorbent resin that unique microvoid structure distributes, and it is technical that macroporous adsorbent resin is referred to removing of agricultural chemicals procymidone, and all can effectively remove take ginseng and American ginseng different parts as the extract of raw material.Have easy and simple to handlely, it is convenient that resin regeneration is processed, and production run cost is low, security good, and the rate of recovery of product is up to more than 92%, and removal effect is good, and the clearance of residual procymidone is more than 90%.
Accompanying drawing explanation
Fig. 1 is the pore structure distribution plan of the embodiment of the present invention 1 and 2 gained macroporous adsorbent resin LKS-11.
Embodiment
Content for a better understanding of the present invention, is described further below in conjunction with specific embodiment.
embodiment 1:
1500mL purified water is joined in the reactor of the 3000ml that thermometer, condensation reflux unit and stirring are housed, in stirring, add 15g gelatin, be warming up to 60 ℃, after gelatin dissolves completely, add well-mixed by 50g vinylbenzene, 450g divinylbenzene, 100g toluene, 100g ethylene dichloride, the mixture of 2.5g benzoyl peroxide composition, form in dispersion medium solution Deng organic mixture after a certain size symmetrical liquid drop, be warming up to 76 ℃, react 5 hours, be warming up to 80 ℃ and solidify 9 hours, stopped reaction.With a large amount of water flushings, sieve, control granularity between 20-70 order, dry, obtain macropore polystyrene resin (ps) Archon.Get Archon 100g, add 600g ethylene dichloride, swelling 2 hours of normal temperature, divides and adds catalyzer aluminum trichloride (anhydrous) (3.33g/30min) for 3 times, is warming up to 80 ℃ of reaction 10h.Cooling, extracts ethylene dichloride out, and washing, packs in apparatus,Soxhlet's, within 12 hours, goes out pore-creating agent with acetone extracting, is washed to without acetone taste, obtains LKS-11 resin.
embodiment 2:
1500mL purified water is joined in the reactor of the 3000ml that thermometer, condensation reflux unit and stirring are housed, in stirring, add 15g gelatin, be warming up to 60 ℃, after gelatin dissolves completely, add well-mixed by 150g vinylbenzene, 350g divinylbenzene, 200g toluene, the mixture of 2.5g benzoyl peroxide composition, form in dispersion medium solution Deng organic mixture after a certain size symmetrical liquid drop, be warming up to 76 ℃, react 5 hours, be warming up to 80 ℃ and solidify 9 hours, stopped reaction.With a large amount of water flushings, sieve, control granularity between 20-70 order, dry, obtain macropore polystyrene resin (ps) Archon.Get Archon 100g, add 600g ethylene dichloride, swelling 2 hours of normal temperature, divides and adds catalyzer FERRIC CHLORIDE ANHYDROUS (6.67g/30min) for 3 times, is warming up to 80 ℃ of reaction 10h.Cooling, extracts ethylene dichloride out, and washing, packs in apparatus,Soxhlet's, within 12 hours, goes out pore-creating agent with acetone extracting, is washed to without acetone taste, obtains LKS-11 resin.
The pore structure data of LKS-11 resin prepared by table 1 embodiment 1 and embodiment 2
| Resin | Specific surface area (m 2/g） | Pore volume (cm 3/g） | Aperture (nm) |
| Embodiment 1 | 1049 | 0.738 | 2.811 |
|
|
1073 | 0.751 | 2.795 |
embodiment 3:
Precision takes LKS11 resin (embodiment 1) and is placed in appropriate vessel, first uses after 95% alcohol immersion 24 h, is washed till without alcohol taste with distilled water.Wash after most alcohol taste with more than 10% NaOH solution soaking 3 h, be then washed till neutrality with distilled water; More than finally using 10% HCl solution soaking 3 h, distilled water is washed till neutrality, and resin wet method good pre-treatment is loaded in post.Precision takes Radix Ginseng extract 20.00 g, adds 200 mL distilled water to stir to leave standstill after 2 h fully to mix and make 0.1 g/mL sample solution.The sample solution that pipettes 2 times of resin volumes is added in resin column, and more than absorption 1 h, coutroi velocity 2～5 mL/min cross post.First wash with the distilled water of 1 times of resin volume, then use 50% ethanol elution of 6 times of resin volumes, collect elutriant.Sealing evaporation equipment reclaims ethanol, and the sample aqueous solution after recovery solvent carries out vacuum drying treatment and obtains the residual product of low procymidone.
embodiment 4:
Precision takes LKS11 resin (embodiment 1) and is placed in appropriate vessel, first uses after 75% alcohol immersion 24 h, is washed till without alcohol taste with distilled water.Wash after most alcohol taste with more than 4% NaOH solution soaking 3 h, be then washed till neutrality with distilled water; More than finally using 6% HCl solution soaking 3 h, distilled water is washed till neutrality.Resin wet method good pre-treatment is loaded in post.Precision takes Radix Panacis Quinquefolii extract 10.00 g, adds 20 mL distilled water to stir to leave standstill after 2 h fully to mix and make 0.1 g/mL sample solution.The sample solution that pipettes 7 times of resin volumes is added in resin column, and more than absorption 1 h, coutroi velocity 2～5 mL/min cross post.First wash with the distilled water of 3 times of resin volumes, then use 85% ethanol elution of 5 times of resin volumes, collect elutriant.Sealing evaporation equipment reclaims ethanol, and the sample aqueous solution after recovery solvent carries out frozen drying processing and obtains the residual product of low procymidone.
embodiment 5:
Precision takes LKS11 resin (embodiment 1) and is placed in appropriate vessel, first uses after 85% alcohol immersion 24 h, is washed till without alcohol taste with distilled water.Wash after most alcohol taste with more than 5% NaOH solution soaking 3 h, be then washed till neutrality with distilled water; More than finally using 5% HCl solution soaking 3 h, distilled water is washed till neutrality, and resin wet method good pre-treatment is loaded in post.Precision takes stem and leaf of Radix Ginseng total saponins 20.00 g and is dissolved in distilled water and stirs to leave standstill after 2 h and fully mix and make 0.01 g/mL sample solution.The sample solution that pipettes 6 times of resin volumes is added in resin column, and more than absorption 1 h, coutroi velocity 2～5 mL/min cross post.First wash with the distilled water of 4 times of resin volumes, then use 75% ethanol elution of 6 times of resin volumes, collect elutriant.Sealing evaporation equipment reclaims ethanol, and the sample aqueous solution after recovery solvent carries out spray drying treatment and obtains the residual product of low procymidone.
embodiment 6:
Precision takes LKS11 resin (embodiment 2) and is placed in appropriate vessel, first uses after 95% alcohol immersion 24 h, is washed till without alcohol taste with distilled water.Wash after most alcohol taste with more than 8% NaOH solution soaking 3 h, be then washed till neutrality with distilled water; More than finally using 10% HCl solution soaking 3 h, distilled water is washed till neutrality, and resin wet method good pre-treatment is loaded in post.Precision takes stem and leaf of Radix Panacis Quinquefolii total saponins 100.00 g and is dissolved in distilled water and stirs to leave standstill after 2 h and fully mix and make 0.05 g/mL sample solution.The sample solution that pipettes 4 times of resin volumes is added in resin column, and more than absorption 1 h, coutroi velocity 2～5 mL/min cross post.First wash with the distilled water of 1 times of resin volume, then use 30%～95% ethanol elution of 7 times of resin volumes, collect elutriant.Sealing evaporation equipment reclaims ethanol, and the sample aqueous solution after recovery solvent carries out frozen drying processing and obtains the residual product of low procymidone.
embodiment 7:
Precision takes LKS11 resin (embodiment 2) and is placed in appropriate vessel, first uses after 80% alcohol immersion 24 h, is washed till without alcohol taste with distilled water.Wash after most alcohol taste with more than 5% NaOH solution soaking 3 h, be then washed till neutrality with distilled water; More than finally using 5% HCl solution soaking 3 h, distilled water is washed till neutrality, and resin wet method good pre-treatment is loaded in post.Precision takes ginseng fruit saponins 10.00 g and is dissolved in distilled water and stirs to leave standstill after 2 h and fully mix and make 0.1 g/mL sample solution.The sample solution that pipettes 3 times of resin volumes is added in resin column, and more than absorption 1 h, coutroi velocity 2～5 mL/min cross post.First wash with the distilled water of 4 times of resin volumes, then use 45% ethanol elution of 4 times of resin volumes, collect elutriant.Sealing evaporation equipment reclaims ethanol, and the sample aqueous solution after recovery solvent carries out spray drying treatment and obtains the residual product of low procymidone.
embodiment 8:
Precision takes LKS11 resin (embodiment 2) and is placed in appropriate vessel, first uses after 90% alcohol immersion 24 h, is washed till without alcohol taste with distilled water.Wash after most alcohol taste with more than 7% NaOH solution soaking 3 h, be then washed till neutrality with distilled water; More than finally using 6% HCl solution soaking 3 h, distilled water is washed till neutrality, and resin wet method good pre-treatment is loaded in post.Precision takes general saponin of gen-seng fruit 12.00 g and is dissolved in distilled water and stirs to leave standstill after 2 h and fully mix and make 0.05 g/mL sample solution.The sample solution that pipettes 6 times of resin volumes is added in resin column, and more than absorption 1 h, coutroi velocity 2～5 mL/min cross post.First wash with the distilled water of 2 times of resin volumes, then use 65% ethanol elution of 5 times of resin volumes, collect elutriant.Sealing evaporation equipment reclaims ethanol, and the sample aqueous solution after recovery solvent carries out vacuum and heating drying processing and obtains the residual product of low procymidone.
Procymidone clearance and the total saponins rate of recovery in table 2, different sources sample
Claims (5)
1. a superhigh cross-linking macroporous adsorbent resin, is characterized in that structural formula is as follows:
(wherein, n=1,2,3 ...).
2. the preparation method of superhigh cross-linking macroporous adsorbent resin as claimed in claim 1, comprises the steps:
1) macroporous polystyrene Archon preparation
Take by weight styrene monomer 10-30, linking agent 70-90, pore-creating agent 50-150, polymerization starter 0.5-1.5, said components is placed in to dispersion medium together, under 60-100 ℃ of condition, react suspension polymerization in 12-20 hour and obtain macroporous polystyrene Archon;
2) crosslinking reaction after
Step (1) gained macroporous polystyrene Archon is joined in swelling agent, under room temperature swelling 2 hours, add catalyzer Lewis acid, at 70-120 ℃, carry out Friedel-Crafts alkylated reaction, reaction times is 8-16 hour, obtains macroporous adsorbent resin.
3. the preparation method of superhigh cross-linking macroporous adsorbent resin as claimed in claim 1, is characterized in that:
Styrene monomer 20, linking agent 80, pore-creating agent 100, polymerization starter 1 in step 1); Temperature of reaction is 70-90 ℃, and the reaction times is 14-18 hour;
Step 2) temperature of reaction is 80-100 ℃, the reaction times is 10-14 hour.
4. the preparation method of superhigh cross-linking macroporous adsorbent resin as claimed in claim 1, is characterized in that:
Styrene monomer described in step 1) is selected from the one in vinylbenzene, vinyl toluene, alpha-methyl styrene, ethyl styrene, optimization styrene;
Described linking agent is selected from multi-vinyl monomer, as divinylbenzene, methacrylate ethylene glycol, trimethylolpropane trimethacrylate, and preferably divinylbenzene;
Described pore-creating agent is selected from aromatic hydrocarbons as toluene, dimethylbenzene; Higher alcohols is as butanols, hexanol, and alkanes is as normal heptane, ethylene dichloride, 200
#gasoline, whiteruss, solid paraffin, ester class is as butylacetate, ethyl acetate, preferably toluene and gasoline, pore-creating agent can use separately or any two to three kinds mix and use, aromatic hydrocarbons is classified 2:1-1:2 as with the ratio of alkanes;
Described polymerization starter is selected from organo-peroxide, as peroxidation paraphenylene terephthalamide, peroxide-2-ethyl hexanoic acid tert-butyl, peroxidation-2 ethyl hexanoic acid tert-pentyl ester etc., and preferably peroxidation paraphenylene terephthalamide;
Described dispersion agent is selected from gelatin or polyvinyl alcohol or Natvosol, and consumption is the 0.5%-2% of dispersion medium weight;
Step 2) described Lewis acid is selected from Zinc Chloride Anhydrous, aluminum trichloride (anhydrous), FERRIC CHLORIDE ANHYDROUS or anhydrous stannic chloride, and the consumption of catalyzer is the 10%-40% of macroporous polystyrene Archon total amount;
Described swelling agent is selected from ethylene dichloride or oil of mirbane, and consumption is 4-8 times of macroporous polystyrene Archon weight.
5. resin method is removed the residual method of procymidone in ginseng, Radix Panacis Quinquefolii extract, comprises the following steps:
1) resin pre-treatment: LKS11 resin prepared by claim 2 is first used after 30%～95% alcohol immersion 24 h, is washed till without alcohol taste with distilled water; After washing most alcohol taste, use 1%-10% NaOH solution soaking 3 ~ 5 hours, be then washed till neutrality with distilled water; Finally use 1%-10% HCl solution soaking 3 ~ 5 hours, distilled water is washed till neutrality;
2) dress post: resin wet method good pre-treatment is loaded in post;
3) sample solution preparation: take pending sample water-soluble, leave standstill and it was fully dissolved in 2 ~ 5 hours after stirring, be made into the sample solution that concentration is 0.05～0.1 g/mL;
4), absorption: the sample solution that pipettes 1～10 times of resin volume is added in resin column, adsorbs 1 ~ 2 hour, and coutroi velocity 2～5 mL/min cross post;
5), desorb: first wash with the distilled water of 1～4 times of resin volume, then use 30%～95% ethanol elution of 1～10 times of resin volume, collect elutriant;
6) reclaim reagent;
7) dry: the sample aqueous solution after recovery solvent carries out drying treatment and obtains the residual product of low procymidone.
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| CN105168281A (en) * | 2015-08-31 | 2015-12-23 | 天津大学 | Method for removing procymidone in ginsenoside through macroreticular resin adsorption-supercritical CO2 elution |
| CN105273138A (en) * | 2015-11-25 | 2016-01-27 | 蚌埠市天星树脂有限责任公司 | Super-large specific surface area adsorbent resin and preparation method thereof |
| CN105777841A (en) * | 2016-04-08 | 2016-07-20 | 赣州禾绿康健生物技术有限公司 | Method for removing propamocarb in araliaceae saponin extract |
| CN109012634A (en) * | 2018-08-16 | 2018-12-18 | 福建农林大学 | NKA macroporous absorbent resin filler pre-treatment method |
| CN110898091A (en) * | 2019-12-18 | 2020-03-24 | 宁波杰顺生物科技有限公司 | Ginseng extract and preparation method thereof |
| CN110960459A (en) * | 2019-12-18 | 2020-04-07 | 宁波杰顺生物科技有限公司 | Grape seed extract and preparation method thereof |
| CN112358563A (en) * | 2020-12-01 | 2021-02-12 | 西安蓝深环保科技有限公司 | Macroporous adsorption resin for lincomycin extraction and synthetic method thereof |
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| CN105168281A (en) * | 2015-08-31 | 2015-12-23 | 天津大学 | Method for removing procymidone in ginsenoside through macroreticular resin adsorption-supercritical CO2 elution |
| CN105168281B (en) * | 2015-08-31 | 2019-12-06 | 天津大学 | method for removing procymidone in ginsenoside through macroporous adsorption resin adsorption-supercritical CO2 elution |
| CN105273138A (en) * | 2015-11-25 | 2016-01-27 | 蚌埠市天星树脂有限责任公司 | Super-large specific surface area adsorbent resin and preparation method thereof |
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| CN112358563B (en) * | 2020-12-01 | 2023-04-25 | 西安蓝深新材料科技股份有限公司 | Macroporous adsorption resin for lincomycin extraction and synthesis method thereof |
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