CN112791110A - Preparation method of ginseng root extract with low pesticide residue - Google Patents

Preparation method of ginseng root extract with low pesticide residue Download PDF

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CN112791110A
CN112791110A CN202110386150.0A CN202110386150A CN112791110A CN 112791110 A CN112791110 A CN 112791110A CN 202110386150 A CN202110386150 A CN 202110386150A CN 112791110 A CN112791110 A CN 112791110A
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pesticide residue
ginseng
extract
root extract
ethanol
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徐宝顺
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Nanjing Qiaokang Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/25Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258Panax (ginseng)
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/003Filters in combination with devices for the removal of liquids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Mycology (AREA)
  • Biotechnology (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to the technical field of biological medicine, and discloses a preparation method of a ginseng root extract with low pesticide residue, which comprises the following steps of S1: firstly, selecting and cleaning ginseng raw materials, shearing roots of the ginseng raw materials, crushing the ginseng raw materials into coarse powder by a crusher, and then adding water for mixing to obtain a primary solution to be extracted; step S2: performing adsorption treatment, specifically, performing macroporous resin D101 adsorption on the obtained extract, resolving with ethanol, filtering with a plate frame, and concentrating; step S3: pesticide residue removal treatment, namely adding water to dilute the obtained concentrated solution, removing pesticide residues by using resin, and then performing secondary concentration treatment; step S4: and (5) preparing a finished product, namely drying the secondary concentrated solution obtained in the step S3 in vacuum, crushing, and finally sieving to obtain a finished product of the extract. The technical scheme can provide the preparation method of the ginseng root extract with low pesticide residue, which has high treatment efficiency for removing pesticide residue and low organic solvent residue content, and the ginsenoside content of the ginseng extract is not lower than 55 percent by HPLC.

Description

Preparation method of ginseng root extract with low pesticide residue
Technical Field
The invention relates to the technical field of biological medicine preparation, in particular to a preparation method of a ginseng root extract with low pesticide residue.
Background
With the development of agricultural industrialization, the production of agricultural products increasingly depends on exogenous substances such as antibiotics and organic pesticides, and the use of a large amount of pesticides inevitably causes the problem of exceeding the standard of pesticide residues of the agricultural products, influences the edible safety of consumers and seriously threatens the lives of the consumers. In addition, many countries have strict limits on the pesticide residues in natural plant products, and the overproof pesticide residues directly influence the export and earning foreign exchange of the products, thereby causing trade problems.
The discovered active ingredients of the total saponins in the ginseng stems and leaves mainly comprise ginsenoside, which has the effects of nourishing and strengthening, soothing the nerves and improving intelligence and enhancing immunity and has good effects on cardiovascular diseases, tumors, inflammations, digestive tract ulcers and other diseases.
At present, the traditional Chinese medicinal materials have various diseases and insect pests, serious damage and large loss, if more than 40 infectious diseases and insect pests are known in ginseng, more than 20 diseases and insect pests occur frequently, chemical pesticides are basically adopted for prevention, and the traditional Chinese medicinal materials are sprayed for 20-30 times per year on average. The university of Shanghai medicine has generally checked the pesticide residue of more than 300 traditional Chinese medicines all over the country, and as a result, all samples contain sixty-six, and most of the samples contain residual amount of dichlorodiphenyl trichloroethane.
Therefore, the problem needs to be solved as early as possible, most of ginseng extract pesticide residues exceed the standard, and the pesticide residues are treated by repeatedly extracting with normal hexane in part at present, but the effect is very little, and the problems of incomplete treatment, high cost, complex process and poor operability exist.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a ginseng root extract with low pesticide residue, which can meet the EC396 standard, has high treatment efficiency for removing pesticide residue and low organic solvent residue content, and simultaneously has the ginsenoside content of the ginseng extract not less than 55 percent by HPLC.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of a ginseng root extract with low pesticide residue comprises the following steps:
step S1: extracting, namely selecting cleaned ginseng raw materials, shearing roots of the ginseng raw materials, crushing the ginseng raw materials into coarse powder by a crusher, and adding water in proportion to obtain a primary solution to be extracted;
step S2: performing adsorption treatment, specifically, performing macroporous resin D101 adsorption on the extract obtained in the step S1, resolving with ethanol, filtering with a plate frame, and concentrating for use in the subsequent steps;
step S3: pesticide residue removal treatment, namely adding water to dilute the concentrated solution obtained in the step S2, removing pesticide residue by using resin, and then performing secondary concentration treatment;
step S4: and (5) preparing a finished product, namely drying the secondary concentrated solution obtained in the step S3 in vacuum, crushing, and finally sieving to obtain a finished product of the extract.
As a further improvement of the invention, the mass ratio of the ginseng raw material to the water in the step S1 ranges from 3:100 to 4:100, the mixing temperature is 90 ℃, and the mixing time is 0.5 to 1 hour.
As a further improvement of the invention, in the step S1, the fineness of the crushed material obtained by crushing through a crusher is 20-30 meshes.
As a further improvement of the invention, the ethanol concentration used in the step S2 is 60-90%, the volume ratio of the ethanol to the macroporous resin D101 is 3.5:1, the ethanol elution flow rate is 500L/h, 3-4 hours are needed, a 500-mesh filter membrane is used for plate-frame filtration, and the ethanol is removed through evaporation concentration.
As a further improvement of the invention, the volume ratio of the solution diluted by adding water to the resin in the step S3 is 1:10, the temperature is controlled at 30-40 ℃, and evaporation dehydration is performed.
As a further improvement of the invention, the vacuum drying temperature in the step S4 is controlled to be 70-80 ℃.
Due to the application of the technical scheme, the technical scheme of the invention has the following beneficial effects: the ginseng raw material is crushed and dissolved by adding water, macroporous resin D101 is selected for adsorption and then is resolved by ethanol, plate-frame filtration is also carried out, then the ginseng raw material is concentrated and refined and then is diluted by water, and the full removal of pesticide residues is realized by carrying out adsorption treatment on the resin again, so that the pesticide residues can be completely adsorbed on the resin, and the effective component saponin is fully extracted, namely the content of the effective component ginsenoside is not lower than the index of 55 percent HPLC, therefore, the ginseng pesticide composition has the beneficial technical effects of low pesticide residue content of the final product, high harmful component removal rate, good product safety and no organic solvent residue; according to the technical scheme, the preparation method adopts a plurality of steps to be matched and processed according to the sequence, and the technical effects of convenience in operation, thorough removal of harmful substances, more environmental protection and high efficiency and capability of meeting the index requirements of various products are achieved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a ginseng root extract with low pesticide residue and a preparation method thereof comprise the following steps:
(1) extraction: selecting ginseng, taking roots of the ginseng, crushing the ginseng into coarse powder of 20-30 meshes, weighing 100g of the coarse powder, adding 2500ml of water, and keeping the temperature at about 90 ℃ for 30 min-1 h;
(2) adsorption: adsorbing the extract obtained in the step (1) by using macroporous resin D101, resolving by using ethanol with the concentration of 70%, wherein the ethanol: the volume ratio of the resin is 3.5:1, the flow rate is 500L/h, 3-4 hours are needed, a 500-mesh filter membrane is used for plate-frame filtration, evaporation concentration is carried out, and ethanol is removed;
(3) removing pesticide residues: diluting the concentrated solution obtained in the step (2) with water, removing pesticide residues with resin, and diluting the product with water: the volume ratio of the resin is 1:10, the temperature is controlled to be 30-40 ℃, and evaporation dehydration is carried out;
(4) and (3) finished product: and (4) carrying out vacuum drying on the concentrated solution obtained in the step (3), wherein the vacuum drying temperature is 70-80 ℃, crushing, and sieving to obtain a finished product.
Example 2:
a ginseng root extract with low pesticide residue and a preparation method thereof comprise the following steps:
(1) extraction: selecting ginseng, taking roots of the ginseng, crushing the ginseng into coarse powder of 20-30 meshes, weighing 100g of the coarse powder, adding 2500ml of water, and keeping the temperature at about 90 ℃ for 30 min-1 h;
(2) adsorption: adsorbing the extract obtained in the step (1) by using macroporous resin LKC36, resolving by using ethanol with the concentration of 70%, and performing ethanol: the volume ratio of the resin is 3.5:1, the flow rate is 500L/h, 3-4 hours are needed, a 500-mesh membrane is used for plate-frame filtration, evaporation concentration is carried out, and ethanol is removed;
(3) removing pesticide residues: diluting the concentrated solution obtained in the step (2) with water, removing pesticide residues with resin, and diluting the product with water: the volume ratio of the resin is 1:10, the temperature is controlled to be 30-40 ℃, and evaporation dehydration is carried out;
(4) and (3) finished product: and (4) carrying out vacuum drying on the concentrated solution obtained in the step (3), wherein the vacuum drying temperature is 70-80 ℃, crushing, and sieving to obtain a finished product.
Example 3:
a ginseng root extract with low pesticide residue and a preparation method thereof comprise the following steps:
(1) extraction: selecting ginseng, taking roots of the ginseng, crushing the ginseng into coarse powder of 20-30 meshes, weighing 100g of the coarse powder, adding 2500ml of water, and keeping the temperature at about 90 ℃ for 30 min-1 h;
(2) adsorption: adsorbing the extract obtained in the step (1) by using mixed macroporous resin D101 and LKC36, resolving by using 70% of ethanol concentration: the volume ratio of the resin is 3.5:1, the flow rate is 500L/h, 3-4 hours are needed, a 500-mesh membrane is used for plate-frame filtration, evaporation concentration is carried out, and ethanol is removed;
(3) removing pesticide residues: diluting the concentrated solution obtained in the step (2) with water, removing pesticide residues with resin, and diluting the product with water: the volume ratio of the resin is 1:10, the temperature is controlled to be 30-40 ℃, and evaporation dehydration is carried out;
(4) and (3) finished product: and (4) carrying out vacuum drying on the concentrated solution obtained in the step (3), wherein the vacuum drying temperature is 70-80 ℃, crushing, and sieving to obtain a finished product.
The detection indexes of the ginsenoside content and pesticide residue content in the ginseng stem and leaf extract are shown in the table below.
Figure 461355DEST_PATH_IMAGE001
The above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.

Claims (6)

1. A preparation method of a ginseng root extract with low pesticide residue is characterized by comprising the following steps:
step S1: extracting, namely selecting cleaned ginseng raw materials, shearing roots of the ginseng raw materials, crushing the ginseng raw materials into coarse powder by a crusher, and adding water in proportion to obtain a primary solution to be extracted;
step S2: performing adsorption treatment, specifically, performing macroporous resin D101 adsorption on the extract obtained in the step S1, resolving with ethanol, filtering with a plate frame, and concentrating for use in the subsequent steps;
step S3: pesticide residue removal treatment, namely adding water to dilute the concentrated solution obtained in the step S2, removing pesticide residue by using resin, and then performing secondary concentration treatment;
step S4: and (5) preparing a finished product, namely drying the secondary concentrated solution obtained in the step S3 in vacuum, crushing, and finally sieving to obtain a finished product of the extract.
2. The method for preparing ginseng root extract with low pesticide residue as claimed in claim 1, wherein the method comprises the following steps: and the vacuum drying temperature in the step S4 is controlled to be 70-80 ℃.
3. The method for preparing ginseng root extract with low pesticide residue as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the ginseng raw material to the water in the step S1 ranges from 3:100 to 4:100, the mixing temperature is 90 ℃, and the mixing time is 0.5 to 1 hour.
4. The method for preparing ginseng root extract with low pesticide residue as claimed in claim 1, wherein the method comprises the following steps: and in the step S1, the fineness of the crushed material is 20-30 meshes.
5. The method for preparing ginseng root extract with low pesticide residue as claimed in claim 1, wherein the method comprises the following steps: the concentration of the ethanol used in the step S2 is 60-90%, the volume ratio of the ethanol to the macroporous resin D101 is 3.5:1, the elution flow rate of the ethanol is 500L/h, 3-4 hours are needed, a 500-mesh filtering membrane is used for plate-frame filtering, and the ethanol is removed through evaporation and concentration.
6. The method for preparing ginseng root extract with low pesticide residue as claimed in claim 1, wherein the method comprises the following steps: and (S3) the volume ratio of the solution diluted by water to the resin is 1:10, the temperature is controlled to be 30-40 ℃, and evaporation dehydration is carried out.
CN202110386150.0A 2021-04-12 2021-04-12 Preparation method of ginseng root extract with low pesticide residue Pending CN112791110A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106086146A (en) * 2016-06-30 2016-11-09 江苏省中国科学院植物研究所 A kind of Preparation method and use of refined precious rare ginsenoside
CN108042590A (en) * 2017-12-29 2018-05-18 杨凌萃健生物工程技术有限公司 A kind of residual extract of Radix Ginseng stem and leaf of low agriculture and preparation method thereof
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
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Patent Citations (6)

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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
CN106086146A (en) * 2016-06-30 2016-11-09 江苏省中国科学院植物研究所 A kind of Preparation method and use of refined precious rare ginsenoside
CN108042590A (en) * 2017-12-29 2018-05-18 杨凌萃健生物工程技术有限公司 A kind of residual extract of Radix Ginseng stem and leaf of low agriculture and preparation method thereof
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
CN111544462A (en) * 2020-06-01 2020-08-18 浙江天草生物科技股份有限公司 Method for removing pesticide residues from ginseng extract

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