CN106581108A - Method for removing residual pesticide propamocarb in ginseng extractive - Google Patents
Method for removing residual pesticide propamocarb in ginseng extractive Download PDFInfo
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- CN106581108A CN106581108A CN201611233903.XA CN201611233903A CN106581108A CN 106581108 A CN106581108 A CN 106581108A CN 201611233903 A CN201611233903 A CN 201611233903A CN 106581108 A CN106581108 A CN 106581108A
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- Prior art keywords
- radix ginseng
- propamocarb
- residual pesticide
- ethyl acetate
- ginseng extract
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for removing residual pesticide propamocarb in ginseng extractive. Compared with the prior art, aiming at the property of propamocarb in ginseng extracting solution, the method comprises the steps of conducting extraction through a mixed solvent of petroleum ether and ethyl acetate, and then conducting filtering through LX-N1 and LX-N2 type macroporous resin and a 40-60-mesh neutral alumina mixture. After treatment, the recovery rate of ginseng total saponins reaches 80%-85%, and the amount of propamocarb is less than 0.01 ppm. The method for removing residual pesticide propamocarb in the ginseng extractive has the advantages of being simple in operation, low in cost and high in recovery rate of ginseng total saponins, and not causing unnecessary loss.
Description
Technical field
The invention belongs to the processing method field of medicinal plant extract, and in particular to remain agriculture in removing Radix Ginseng extract
The method of medicine Propamocarb.
Background technology
The another name of Radix Ginseng is Sphallerocarpus gracilis, Herba Stellariae Saxatilis, SHENCAO, the king of BAICAO, is one of well-known " northeast three essentials-essence ".Radix Ginseng is certainly
Gu is described as the superfine product of " king of BAICAO " " YIN nourishing mends life, strengthening the body resistance ", and containing various Saponins and polysaccharide constituents, leachate can be by skin
Skin slow-absorbing and without pessimal stimulation, can skin expansion blood capillary, promote cutaneous circulation, increase skin-nourishing, adjust
The water and oil balance of skin, prevents skin dehydration, hardening, corrugation, Radix Ginseng active substance from suppressing melanic reducing property, making skin
It is pure white smooth, skin elasticity can be strengthened, obtain cell newborn, it is the superfine product improved looks.Radix Ginseng is directly immersed in into 50% sweet
Oil, glycerol rubs face with the hands after 10 days, or Radix Ginseng is decocted into into extract, and daily past face washing water a bit, with the glycerol containing Radix Ginseng face or people is rubbed with the hands
Ginseng water face-washing, can allow skin quite to moisten.
But the Ginseng Growth cycle is longer, and Radix Ginseng has larger specific surface area and soil directly contact, therefore, wherein
Persticide residue is higher, and Radix Ginseng extract is the product after further concentration, and pesticide residues therein are higher.
Propamocarb is a kind of low toxicity antibacterial with local systemic action, belongs to carbamatess.To Oomycete fungal
There is specially good effect.It remains in soil and is absorbed by Radix Ginseng, and after extraction, concentration is high, is hazardous to the human body.
The method for the residual pesticide in Radix Ginseng being purified in prior art and being removed, during these methods are to removing Radix Ginseng
Organochlorine pesticide has a certain effect, but have that operating pressure is high, equipment investment is big, operating cost is high, ginsenoside's loss etc. lacks
Point.
The content of the invention
It is an object of the invention to provide a kind of method for removing residual pesticide Propamocarb in Radix Ginseng extract, operation letter
Single, low cost, and the Radix Ginseng total saponinss response rate is high, does not cause unnecessary loss.
The method of residual pesticide Propamocarb, comprises the following steps in a kind of removing Radix Ginseng extract that the present invention is provided：
1) mixed extractant solvent of Radix Ginseng extractive solution's petroleum ether and ethyl acetate, removes layered material liquid；
2) then filter；
3) filtrate concentrates, is dried, obtains final product.
Step 1) described in the preparation method of Radix Ginseng extractive solution be：
After Radix Ginseng is crushed, it is added to the water, heated and boiled extracts for the first time 2.5-3.5h；Filtering residue is added in water, heating
Boil second extraction 1.5-2.5h；Feed liquid is extracted twice in merging.
Further, Radix Ginseng is crushed, and crosses 40-60 mesh sieves.
Further, the mass ratio of Radix Ginseng and water is 1 when extracting for the first time:7-10；The matter for extracting Radix Ginseng and water second
Amount is than being 1:5-8.Further, it is described it is concentrated in vacuo be under the conditions of 60 DEG C；Rear filtrate volume concentrated in vacuo is Ginseng Quality
1.5-2.5 times of L/kg.
Further, step 1) in, the mixed solvent petrochina ether and the volume of ethyl acetate of petroleum ether and ethyl acetate
Than for 1:1-2；
Step 1) in extracting solution and petroleum ether and ethyl acetate mixed solvent volume ratio be 1:1-2.
Step 1) in Radix Ginseng extractive solution's petroleum ether and ethyl acetate mixed extractant solvent 8-10 time.
Step 2) described in filter and be specially：
Lower floor's feed liquid after extraction mixes with filter medium, stirring at normal temperature, sucking filtration.
Further, the filter medium be LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral alumina according to
Mass ratio 1.5:1.5:2～2:2:1 mixture.
Further, step 2) in the amount ratio of lower floor's feed liquid and filter medium be 1.5-2.5L：50g.
Further, step 2) in stirring at normal temperature 24h.
Compared with prior art, the present invention is directed to the property of the Propamocarb in Radix Ginseng extractive solution, by petroleum ether and acetic acid
After the mixed solvent of ethyl ester is first extracted, then with LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral alumina aluminium mixture mistakes
Filter, after treatment, the Radix Ginseng total saponinss response rate 80～85%, Propamocarb<0.01ppm.The method operation letter that the present invention is provided
Single, low cost, and the Radix Ginseng total saponinss response rate is high, does not cause unnecessary loss.
Specific embodiment
Embodiment 1
The method of residual pesticide Propamocarb, comprises the following steps in a kind of removing Radix Ginseng extract：
1) Radix Ginseng palpus raw material 1kg is taken, 40-60 mesh is ground into, in being placed into the round-bottomed flask of 15L, 7-10L water is added,
Heating, boils beginning timing certainly, extracts 3 hours, filters, and collects feed liquid；Filtering residue adds 5-8L water, heating, and beginning is boiled certainly
Timing, extracts 2 hours, filters, and collects feed liquid, and feed liquid is extracted twice in merging, concentrated in vacuo under the conditions of 60 DEG C, is obtained Radix Ginseng and is carried
Take liquid product 1.5-2.5L；
2) volume ratio petroleum ether is used：Ethyl acetate=1：1.5 mixed solvent equal-volume room temperature extraction Radix Ginseng extractive solution 8
It is secondary, remove layered material liquid；
3) and then in the lower floor's feed liquid for obtaining LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral aluminas are added
(mass ratio of LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral aluminas is 1.5 to aluminium mixture 50g:1.5:2), often
Temperature stirring 24h, sucking filtration obtains filtrate；
4) filtrate is dried in 60 DEG C of concentrations, you can.
The Radix Ginseng total saponinss response rate 80～85%, Propamocarb<0.01ppm.
Embodiment 2
The method of residual pesticide Propamocarb, comprises the following steps in a kind of removing Radix Ginseng extract：
1) Radix Ginseng palpus raw material 1kg is taken, 40-60 mesh is ground into, in being placed into the round-bottomed flask of 15L, 7-10L water is added,
Heating, boils beginning timing certainly, extracts 3 hours, filters, and collects feed liquid；Filtering residue adds 5-8L water, heating, and beginning is boiled certainly
Timing, extracts 2 hours, filters, and collects feed liquid, and feed liquid is extracted twice in merging, concentrated in vacuo under the conditions of 60 DEG C, is obtained Radix Ginseng and is carried
Take liquid product 1.5-2.5L；
2) volume ratio petroleum ether is used：Ethyl acetate=1：1.5 mixed solvent equal-volume room temperature extraction Radix Ginseng extractive solution 10
It is secondary, remove layered material liquid；
3) and then in the lower floor's feed liquid for obtaining LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral aluminas are added
(mass ratio of LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral aluminas is 2 to aluminium mixture 50g:2:1), room temperature is stirred
24h is mixed, sucking filtration obtains filtrate；
4) filtrate is dried in 60 DEG C of concentrations, you can.
The Radix Ginseng total saponinss response rate 80～85%, Propamocarb<0.01ppm.
Claims (8)
1. it is a kind of removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that methods described include following step
Suddenly：
1) mixed extractant solvent of Radix Ginseng extractive solution's petroleum ether and ethyl acetate, removes layered material liquid；
2) then filter；
3) filtrate concentrates, is dried, obtains final product.
2. it is according to claim 1 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that step
1) in, the mixed solvent petrochina ether of petroleum ether and ethyl acetate and the volume ratio of ethyl acetate are 1:1-2.
3. it is according to claim 1 and 2 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that
Step 1) in extracting solution and petroleum ether and ethyl acetate mixed solvent volume ratio be 1:1-2.
4. it is according to claim 1 and 2 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that
Step 1) in Radix Ginseng extractive solution's petroleum ether and ethyl acetate mixed extractant solvent 8-10 time.
5. it is according to claim 1 and 2 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that
Step 1) described in the preparation method of Radix Ginseng extractive solution be：
After Radix Ginseng is crushed, it is added to the water, heated and boiled extracts for the first time 2.5-3.5h；Filtering residue is added in water, heated and boiled
Extract 1.5-2.5h second；Feed liquid is extracted twice in merging.
6. it is according to claim 5 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that first
The mass ratio of Radix Ginseng and water is 1 during secondary extraction:7-10；The mass ratio for extracting Radix Ginseng and water for second is 1:5-8.
7. it is according to claim 1 and 2 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that
Step 2) described in filter and be specially：
Lower floor's feed liquid after extraction mixes with filter medium, stirring at normal temperature, sucking filtration；
The filter medium is LX-N1, LX-N2 model macroporous resin and 40-60 mesh neutral alumina according to mass ratio 1.5:
1.5:2～2:2:1 mixture.
8. it is according to claim 1 and 2 removing Radix Ginseng extract in residual pesticide Propamocarb method, it is characterised in that
Step 2) in the amount ratio of lower floor's feed liquid and filter medium be 1.5-2.5L：50g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233903.XA CN106581108B (en) | 2016-12-28 | 2016-12-28 | Method for removing residual pesticide propamocarb in ginseng extract |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233903.XA CN106581108B (en) | 2016-12-28 | 2016-12-28 | Method for removing residual pesticide propamocarb in ginseng extract |
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| CN106581108A true CN106581108A (en) | 2017-04-26 |
| CN106581108B CN106581108B (en) | 2020-10-09 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112007380A (en) * | 2020-08-23 | 2020-12-01 | 赣州禾绿康健生物技术有限公司 | Device and method for removing residual dimethomorph in ginsenoside extract |
| CN112028961A (en) * | 2020-08-17 | 2020-12-04 | 赣州禾绿康健生物技术有限公司 | Method and equipment for removing carbendazim in ginsenoside extract |
| CN113698987A (en) * | 2021-08-30 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Method for removing residual pesticide in corn oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103393928A (en) * | 2013-07-29 | 2013-11-20 | 常熟雷允上制药有限公司 | High-capacity pulse-activating injection and preparation method thereof |
| CN103550273A (en) * | 2013-11-04 | 2014-02-05 | 湖南绿蔓生物科技股份有限公司 | Method for extracting low-pesticide-residue ginsenoside from ginsengs |
| CN104490966A (en) * | 2014-12-04 | 2015-04-08 | 宁波中药制药有限公司 | Method for removing pesticide residues in ginseng stem leaf extracts |
| 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 |
-
2016
- 2016-12-28 CN CN201611233903.XA patent/CN106581108B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103393928A (en) * | 2013-07-29 | 2013-11-20 | 常熟雷允上制药有限公司 | High-capacity pulse-activating injection and preparation method thereof |
| CN103550273A (en) * | 2013-11-04 | 2014-02-05 | 湖南绿蔓生物科技股份有限公司 | Method for extracting low-pesticide-residue ginsenoside from ginsengs |
| CN104490966A (en) * | 2014-12-04 | 2015-04-08 | 宁波中药制药有限公司 | Method for removing pesticide residues in ginseng stem leaf extracts |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028961A (en) * | 2020-08-17 | 2020-12-04 | 赣州禾绿康健生物技术有限公司 | Method and equipment for removing carbendazim in ginsenoside extract |
| CN112007380A (en) * | 2020-08-23 | 2020-12-01 | 赣州禾绿康健生物技术有限公司 | Device and method for removing residual dimethomorph in ginsenoside extract |
| CN112007380B (en) * | 2020-08-23 | 2021-10-22 | 赣州禾绿康健生物技术有限公司 | Device and method for removing residual dimethomorph in ginsenoside extract |
| CN113698987A (en) * | 2021-08-30 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Method for removing residual pesticide in corn oil |
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| CN106581108B (en) | 2020-10-09 |
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Denomination of invention: A method for removing residual pesticide shuangmeiwei in ginseng extract Effective date of registration: 20211125 Granted publication date: 20201009 Pledgee: Wuhu Jinsheng Rural Commercial Bank Co.,Ltd. Qingshui sub branch Pledgor: WUHU ACEGEM BIOLOGICAL TECHNOLOGY Co.,Ltd. Registration number: Y2021980013239 |