JP2006089414A - Method for removing residual agricultural chemical of plant extract and plant extract - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for removing a residual agricultural chemical of a plant extract by using carbon dioxide fluid kept in a supercritical or subcritical state, in which the residual agricultural chemical can efficiently be removed without loss or deterioration of a plant extract ingredient. <P>SOLUTION: The method for removing the residual agricultural chemical of the plant extract comprises a carbon dioxide-dissolving step for dissolving carbon dioxide in the plant extract material by bringing the plant extract material into contact with the carbon dioxide fluid, a carbon dioxide supercritical treatment step for retaining the plant extract material in which the carbon dioxide is dissolved in the supercritical or subcritical state and agitating the solution, and a carbon dioxide-removing step for removing carbon dioxide from the plant extract material by rapidly reducing the pressure of the plant extract material to ordinary pressure. In the carbon dioxide-dissolving step, an aspect using the carbon dioxide fluid forming microbubble by passing the carbon dioxide fluid through a mesh-like filter having ≤100 μm mesh is preferable. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for removing residual pesticides from a plant extract using a supercritical or subcritical carbon dioxide fluid, and a plant extract obtained by the method for removing residual pesticides.

  Carbon dioxide supercritical fluid greatly reduces the extraction efficiency in samples containing a large amount of water. However, carbon dioxide supercritical fluid is microbubbled and mixed with a liquid to efficiently extract large quantities at low temperatures. Devices that can do this have been proposed (see Patent Documents 1 and 2).

  From plant extracts extracted from plants with hydroalcoholic alcohol, the pesticides used in the past have been absorbed from the roots by the plants that have accumulated in the soil without being decomposed. May be attached or absorbed and concentrated to detect residual pesticides.

As a method for removing residual agricultural chemicals from such an extract, for example, there are (1) a method for supercritical extraction of dry plant raw materials and (2) a method for extraction with a hydrophobic solvent. However, in the supercritical extraction of (1), since a high-pressure apparatus is used, there is a problem that the amount of the plant dry raw material charged per extraction batch is reduced and a great production cost is required. On the other hand, the extraction with the hydrophobic solvent (2) requires a large amount of heat when recovering the solvent remaining in the plant raw material, resulting in significant energy consumption and quality deterioration such as browning, and residual agricultural chemicals. There is a risk of extracting and losing components with similar physical properties.
Further, the plant extract is dissolved in a mixture of a lower aliphatic alcohol and water having a volume ratio of 10:90 to 80:20, and the resulting solution is porous with a pore having a most frequent radius of 30 to 120 mm. There has been proposed a method for removing residual agricultural chemicals in a plant extract by bringing the residual agricultural chemicals in a solution into contact with an adsorption resin and adsorbing the residual agricultural chemicals in the adsorption resin and recovering the plant extract from the treated solution (Patent Document 3). reference). However, even in this method, there is a problem that an extraction component having properties close to those of the residual agricultural chemical has a large adsorption loss and the yield of the extract is lowered.

  Therefore, there is a strong demand for the development of a method for efficiently removing residual agricultural chemicals without loss or deterioration of plant extract components.

JP 2001-128652 A JP 2001-299303 A JP 2000-72790 A

  This invention is made | formed in view of this present condition, and makes it a subject to solve the said various problems in the past and to achieve the following objectives. That is, according to the present invention, residual pesticides can be efficiently removed from the plant extract material by bringing a supercritical or subcritical carbon dioxide fluid into contact with the plant extract material, and the loss or deterioration of the plant extract component is reduced. An object of the present invention is to provide a method for removing residual agricultural chemicals from a plant extract and a plant extract that can be continuously extracted at low temperature, can be mass-produced, and can achieve a significant cost reduction.

As a result of intensive studies by the present inventors in order to solve the above problems, the following knowledge has been obtained. That is, it was found that residual pesticides can be efficiently removed by liquid-liquid extraction by contacting the plant extract material with carbon dioxide supercritical fluid.
Further, the carbon dioxide supercritical fluid can be microbubbled to reach the saturation concentration of carbon dioxide in a short time. Furthermore, the extraction efficiency is dramatically increased by using the reaction coil, and after the plant extraction raw material is efficiently extracted on a large scale by alcohol extraction without drying and directly extracting as in the conventional method, the liquid-liquid By performing supercritical extraction, the diffusive and cohesive properties of supercritical fluids can be utilized to the maximum, so that there is no loss or deterioration of plant extract components, and pesticide residues can be efficiently removed from plant extracts. I found out.

The present invention is based on the above findings of the present inventors, and means for solving the above problems are as follows. That is,
<1> A carbon dioxide gas dissolving step in which a plant extract material is brought into contact with a carbon dioxide gas fluid to dissolve the carbon dioxide gas fluid in the plant extract material, and a plant extract material in which the carbon dioxide gas is dissolved is supercritical to carbon dioxide gas. A carbon dioxide supercritical treatment step of maintaining and stirring in a subcritical state, and a carbon dioxide gas removal step of rapidly reducing the plant extract material to normal pressure to remove carbon dioxide from the plant extract material. A method for removing residual pesticides from plant extracts.
<2> The method for removing residual pesticides from a plant extract according to <1>, wherein in the carbon dioxide gas dissolving step, carbon dioxide gas fluid that is microbubbled through a mesh filter having a mesh size of 100 μm or less is used.
<3> A plant extract obtained by extracting a plant extract raw material with water, a hydrophilic solvent, and a mixed solvent thereof, and a plant extract obtained by extracting the plant extract with water, a hydrophilic solvent, and these The method for removing residual agricultural chemicals from a plant extract according to any one of <1> to <2>, wherein the plant extract solution is any one of plant extract solutions dissolved in any of mixed solvents.
<4> Plant extract material is a plant extract obtained by extracting a plant extract raw material with water, ethanol, or a mixed solvent thereof, and a plant extract is dissolved with water, ethanol, or a mixed solvent thereof. It is a residual agrochemical removal method of the plant extract as described in said <3> which is either a plant extract solution.
<5> A plant extract obtained by the method for removing residual agricultural chemicals according to any one of <1> to <4>.

  According to the present invention, various problems in the prior art can be solved, liquid-liquid extraction can be miniaturized as continuous extraction by contacting the plant extraction material with carbon dioxide supercritical fluid, loss of plant extraction components at low cost It can be efficiently removed from plant extracts and can be suitably used in various fields such as food additives, cosmetic constituents, pharmaceuticals, and quasi drugs.

(Residual pesticide removal method of plant extract and plant extract)
The method for removing residual agricultural chemicals from plant extracts of the present invention comprises a carbon dioxide gas dissolving step, a carbon dioxide supercritical treatment step, and a carbon dioxide removing step, and further comprising other steps as necessary.
The plant extract of the present invention is obtained by the method for removing residual agricultural chemicals of the plant extract of the present invention.
Hereinafter, the details of the plant extract of the present invention will be clarified through the description of the method for removing residual agricultural chemicals of the plant extract of the present invention.

  Here, in the residual pesticide removal method of the plant extract of the present invention, the pesticide that can be removed is not particularly limited and can be appropriately selected according to the purpose. For example, EPN, EPTC, p, p- DDD, p, p-DDE, α-BHC, β-BHC, γ-BHC, δ-BHC, acrinathrin, acetamiprid, acephate, isofenphos, isofenphos P = O, isoprocarb, iprodione, imibenconazole, edifenphos, esprocarb, etiophencarb , Ethophos, etrimfos, kazusafos, captahol, carbaryl, quinalphos, quinomethionate, captan, chlorpyrifos, chlorfenvinphos, chlorbenzilate, chloropropham, dietofencarb, diclofuranide, dichlorvos, dicoho , Cyhalothrin, diphenoconazole, cyfluthrin, cyproconazole, cypermethrin, dimethipine, dimethylvinphos, silafluophene, diazinon, thiobencarb, thiomethone, deltamethrin, tenylchlor, tebuconazole, tebufenpyrad, tefluthrin, terbufos, triazimenol trichlorate Phosmethyl, paclobutrazol, parathion, parathion methyl, halfenprox, viteltanol, pyraclophos, pyridaben, pyrifenox-E, pyrifenox-Z, pyriproxyfen, pirimicarb, pyrimidifen, pyrimiphosmethyl, phenarimol, fenitrothion, phenocarb , Fensulfothion, fenthion, phentoate, fenvalerate, butyre , Flucitrinate, flutolanil, fulvalinate, flusilazole, pretilachlor, prothiophos, propiconazole, permethrin, bendiocarb, pendimethalin, benfrate, hosalon, phostiazate, malathion, microbutanyl, methamidophos, methiocarb, metolachlor, mefenaset, Examples include mepronil, lenacyl, etofenprox, oxadixyl, chlorfenapyr, chlorothalonil, fenpropatron, fusalide, butamifos, buprofezin, fludioxonyl, cresoxime methyl, procymidone, mesomil, metalaxyl, methidathion, azoxystrobin, and the like.

-Carbon dioxide dissolution process-
The carbon dioxide gas dissolving step is a step of bringing the plant extract material into contact with a carbon dioxide fluid to dissolve the carbon dioxide fluid in the plant extract material.
The carbon dioxide gas dissolving step is preferably performed under carbon dioxide saturation conditions of a temperature of 0 to 30 ° C. and a pressure of 10 to 30 MPa.
In the carbon dioxide gas dissolving step, using a carbon dioxide gas fluid that is micro-bubbled through a mesh filter having a mesh of 100 μm or less improves the solubility of the carbon dioxide gas in the plant extract material, so that the carbon dioxide gas has a saturated concentration. It is preferable in terms of increasing the contact efficiency. It is more preferable to use a mesh filter having a mesh of 20 μm or less.
In addition, the contact efficiency between the plant extract material and carbon dioxide can be increased by using a high-speed mixer, an ultrasonic generator, or the like.

  There is no restriction | limiting in particular as said plant extraction raw material, According to the objective, it can select suitably, For example, (1) The plant extraction raw material is extracted with water, a hydrophilic solvent, and these mixed solvents. Any of the obtained plant extract and (2) a plant extract solution prepared by dissolving a plant extract in water, a hydrophilic solvent, or a mixed solvent thereof is preferable.

  The plant extraction raw material is not particularly limited and may be appropriately selected depending on the purpose.For example, Maria thistle, Ponkan, thistle, Achacha, opium, aloe bear, ginkgo, fennel, turmeric, usbeneer, moths, ages Ezoukogi, Life-saving grass, Yellow spirit, Ougi, Ogon, Obakaku, Barley, Hypericum grass, Persimmon, Camille, Licorice, Kidachi aloe, Gymnema, Cabbage, Jade bamboo, Quillaja, Gold-silver flower, Chrysanthemum flower, Ginkgo, Red ginseng, Ginseng, Bear bear, Mulberry, Laurel Leaves, Seiko, Gentiana, Wheat, Rice, Burdock, Sesame, Salvia, Sanza, Shiso, Sanshishi, Sanche, Sanroku, Sanyaku, Shiitake, Murasakihime, Glaze, Car Forage, Ginger, White Ginger, Horsetail, Stevia, senkyu, senna, assembly, buckwheat, radish, tiso, soy, tamarind, cod, chimpi, toll, tomato Liu, Cordyceps, Corn, Sashimi, Ginseng, Shinobi Winter, Parsley, Beach Windbreak, Hamelis, Himematsu Rin, Bilberry, Biwa, Bukuryo, Grape, Blueberry, Loofah, Hematin, Bodhi Tree, Peony Skin, Hop, Pine Leaf, Peach, Melissa, Yucca, Yokuinin, Artemisia, Rye, Lacanca, Green tea, Apple, Rooibos, Luscus, Ganoderma, Reindeer grass, Rosehip, Rosemary and the like.

  The extraction treatment is not particularly limited and may be appropriately selected from known methods according to the purpose. Examples thereof include extraction treatment with water, hot water, a hydrophilic organic solvent, and the like. As a solvent used for extraction, it is preferable to use water, a hydrophilic organic solvent, or a mixture thereof at room temperature or a temperature not higher than the boiling point of the solvent.

  Examples of the water include pure water, tap water, well water, mineral spring water, mineral water, hot spring water, spring water, and fresh water, and those obtained by performing various treatments on these. Examples of the treatment applied to water include purification, heating, sterilization, filtration, ion exchange, adjustment of osmotic pressure, buffering, and the like. Therefore, the water that can be used as the extraction solvent in the present invention includes purified water, hot water, ion-exchanged water, physiological saline, phosphate buffer, phosphate buffered saline, and the like.

Examples of the hydrophilic organic solvent include lower alcohols having 1 to 5 carbon atoms such as methanol, ethanol, propyl alcohol, and isopropyl alcohol; lower aliphatic ketones such as acetone and methyl ethyl ketone; 1,3-butylene glycol, propylene glycol, Examples thereof include polyhydric alcohols having 2 to 5 carbon atoms such as glycerin, and a mixed solvent of these hydrophilic organic solvents and water can be used. In addition, when using the mixed solvent of water and a hydrophilic organic solvent, in the case of the said lower alcohol, 1-90 mass parts of lower alcohol is preferable with respect to 10 mass parts of water. In the case of the lower aliphatic ketone, 1 to 40 parts by mass of the lower aliphatic ketone is preferable with respect to 10 parts by mass of water. In the case of the said polyhydric alcohol, 1-90 mass parts of polyhydric alcohol is preferable with respect to 10 mass parts of water.
Among these, a plant extract obtained by extracting a plant extract raw material with water, ethanol, or a mixed solvent thereof, and a plant extract solution obtained by dissolving a plant extract with water, ethanol, or a mixed solvent thereof. Any one of the above is preferable, and either a hydrous ethanol extract of a plant extract raw material or a hydrous ethanol solution of a plant extract obtained by dissolving a hydrous ethanol extract of a plant with hydrous ethanol is particularly preferable.

  In the extraction treatment, for example, a plant extraction raw material is put into a treatment tank filled with an extraction solvent, and left standing for 30 minutes to 2 hours with occasional stirring as necessary to elute soluble components, followed by filtration and solidification. An extract is obtained by removing a thing, distilling an extraction solvent off from the obtained extract, and drying. The amount of extraction solvent is usually 5 to 15 times (mass ratio) of the plant extraction raw material, and the extraction condition is usually about 1 to 4 hours at 50 to 95 ° C. when water is used as the extraction solvent. . Moreover, when using the mixed solvent of water and ethanol as an extraction solvent, it is about 30 minutes-4 hours at 40-80 degreeC normally.

-Carbon dioxide supercritical processing-
The carbon dioxide gas supercritical treatment step is a step of stirring the plant extract material in which the carbon dioxide gas is dissolved while maintaining the carbon dioxide gas in a supercritical to subcritical state.
The carbon dioxide supercritical treatment step is preferably performed while maintaining carbon dioxide supercritical conditions at a temperature of 31.1 to 50 ° C. (preferably 31.5 to 40 ° C.) and a pressure of 10 to 30 MPa. Under this condition, carbon dioxide dissolved in the plant extract material quickly changes to a supercritical state. Supercritical carbon dioxide diffuses and aggregates very efficiently, and residual pesticides can be efficiently removed from the plant extract material by the permeation of carbon dioxide.

-Carbon dioxide removal process-
The carbon dioxide removal step is a step of removing carbon dioxide by rapidly reducing the pressure applied to the plant extract material to normal pressure.
By rapidly reducing the pressure applied to the plant extract material to normal pressure, the carbon dioxide dissolved in the plant extract material is instantaneously expanded and vaporized.

In the present invention, further comprising a recycling step, the separated solute extracted from the carbon dioxide supercritical fluid in the decompression unit is separated, dehydrated with granular activated carbon after carbon sieve dehydration as carbon dioxide, and subjected to pressure liquefaction treatment. It is preferable in that it can be reused later and cost can be reduced.
The method for removing residual pesticides from plant extracts of the present invention described above can efficiently remove residual pesticides from plant extract materials by connecting the steps and continuously treating them.

  Here, as a device for carrying out the method for removing a pesticide residue of a plant extract of the present invention, for example, a microbubble carbon dioxide supercritical treatment device shown in FIG. 1 is preferably exemplified. The details of the microbubble carbon dioxide supercritical processing apparatus are described in Japanese Patent Application Laid-Open Nos. 2001-299303 and 2001-128652.

The microbubble carbon dioxide supercritical processing apparatus shown in FIG. 1 continuously supplies plant extract material from the stock solution supply tank 1 to the dissolution tank 7 by the high-pressure pump 2, and contacts the carbon dioxide gas fluid in the dissolution tank 7.
On the other hand, between the liquid carbon dioxide cylinder 3 and the bottom of the dissolution tank 7, a carbon dioxide gas flow path including a cooler 4, a pump 4, and a heater 6 is provided. Thus, by cooling liquid carbon dioxide gas with a cooler and letting it pass through a pump, the pressure becomes constant, so that a certain amount of carbon dioxide gas can be put into the dissolution tank.

  A mesh filter 9 is provided at the bottom of the dissolution tank 7. The saturated concentration is efficiently reached by contacting and mixing with the liquefied carbon dioxide gas formed into microbubbles through the mesh filter 9 having a mesh of 100 μm or less (preferably a mesh of 20 μm or less). The dissolution tank 7 is maintained at 0 ° C. to 30 ° C., and the pressure is adjusted to 10 Mpa to 30 Mpa, so that the diffusibility reaching the saturated dissolution concentration of carbon dioxide gas is sufficiently exhibited. Then, the contact / mixed solution having reached the saturated concentration is transferred to the reaction coil 8 (holding section) and heated to 31.1 ° C. or higher to bring the carbon dioxide gas into a supercritical state. Extract solutes into Then, a reaction liquid is moved to the gas-liquid separation tank 10, and a plant essential oil extract and a carbon dioxide supercritical fluid are isolate | separated. Since the separation tank is thus provided, the efficiency of the supercritical processing is improved.

Next, the separated carbon dioxide supercritical fluid is separated from the solute extracted in the decompression section, dehydrated with molecular activated carbon after carbon sieve dehydration, and reused through pressure liquefaction treatment. The separated and collected liquid sample is concentrated under reduced pressure and then spray-dried to obtain a powder product.
In FIG. 1, 11 represents a gas-liquid separation sensor, 12 represents a separation tank, 13 represents a trap, and 16 represents a processing sample tank.

According to the method for removing pesticide residues from plant extracts of the present invention, pesticide residues can be efficiently removed from plant extract materials, there is no loss of plant extract components, quality deterioration can be prevented, and continuous extraction processing is possible. Thus, significant cost reduction can be achieved.
The plant extract obtained by the method for removing a pesticide residue of the plant extract of the present invention has almost all the pesticide residue removed, is excellent in safety, and can be widely used for pharmaceuticals, health foods, cosmetics, foods and drinks, etc. .

  Examples of the present invention will be described below, but the present invention is not limited to these examples.

Example 1
-Preparation of Maria Thistle Extract-
1 kg of seeds of Maria Thistle were pulverized and extracted with 10 L of 90 mass% ethanol for 2 hours while circulating at room temperature. After solid-liquid separation on a 100 mesh screen, 10 L of 90% by mass ethanol (mass ratio of water to ethanol 1: 9) was added to the extraction bowl, and extraction was performed at room temperature for 1 hour. Thereafter, solid-liquid separation was performed with a 100 mesh screen. The two extracts were combined and clarified by diatomaceous earth precoat to obtain 18 L of extract. Subsequently, after concentrating the obtained extract under reduced pressure, ethanol was added to prepare 3 L of a 60 mass% ethanol solution. After adding 50 g of activated carbon, the mixture was heated to reflux for 1 hour and clarified to obtain 2.5 L of a Maria Thistle extract.
The solid content of the resulting Maria Thistle extract was 110 g. In addition, the content of silymarin as an active ingredient in the Maria Thistle extract was 31% by mass.

  As a result of measuring the residual agricultural chemical contained in the obtained Maria Thistle extract by GC-MS under the following measuring equipment and conditions, contamination of residual agricultural chemicals of malathion 0.02 ppm and parathion 0.015 ppm was confirmed.

<GC-MS measurement conditions>
Measuring instrument: 6890N GC, 5973MSD manufactured by Agilent
Column: HP-5MS, 0.25 μm × 30 m
Oven: 80 ° C. (2 min) → 30 ° C./min→180° C. (5 min) → 3 ° C./min→260° C. (10 min)
Flow rate: He 1mL / min
Inlet: 250 ° C. Pulsed splitless (pulse pressure 30 psi, 1.5 min purge 1.45 min)
Injection volume: 2 μL
MS: SIM measurement (EI)

-Preparation of Maria Thistle supercritical extract-
The extract of Maria thistle obtained above is liquefied at a sample flow rate of 20 mL / min using the microbubble supercritical processing apparatus shown in FIG. 1 (a mesh filter having a mesh of 100 μm is arranged at the bottom of the dissolution tank 7). Extraction was carried out for 3 hours with a flow rate of carbon dioxide at 20 mL / min, a treatment pressure of 20 Mpa, a dissolution bath temperature of 20 ° C., and a reaction coil holder temperature of 40 ° C. As a result, 108 g of a supercritical extract was obtained. Further, the content of silymarin as an active ingredient in the Maria Thistle supercritical extract was 31% by mass.
About the obtained Maria thistle supercritical extract, the residual pesticide was measured by GC-MS in the same manner as described above. As a result, malathion was not detected and parathion was not detected, and the pesticide was removed. In addition, it was confirmed that the content of silymarin, which is an active ingredient, was not changed by the supercritical extraction treatment.

(Example 2)
-Preparation of Ponkan extract-
To 2500 kg of Ponkan, 50 L of 30% by mass ethanol (mass ratio of water to ethanol: 7: 3) as an extraction solvent was added, and the mixture was heated and extracted at 80 ° C. for 2 hours with a reflux extractor and filtered while hot. The obtained extracts were combined, concentrated under reduced pressure, and further dried to obtain a Ponkan extract.
The obtained extract was treated with column chromatography using Diaion HP-20 (manufactured by Mitsubishi Chemical Corporation) as an adsorption resin, and then eluted with 70% by mass aqueous methanol. The obtained fraction was treated with activated carbon. Furthermore, after concentrating under reduced pressure, it was dried to obtain 1.3 kg of a crude nobiletin product. In addition, the content of nobiletin as an active ingredient in the nobiletin crude purified product was 45% by mass.
As a result of measuring the residual agricultural chemicals contained in the obtained nobiletin crude purified product by GC-MS in the same manner as in Example 1, contamination of residual agricultural chemicals of 0.15 ppm methidathion was confirmed.

-Production of Ponkan supercritical extract-
A solution obtained by dissolving the crude nobiletin product obtained above in 60% by mass of ethanol was used using a microbubble supercritical processing apparatus (a mesh filter having a mesh size of 100 μm disposed at the bottom of the dissolution tank 7) shown in FIG. Then, a sample flow rate of 20 mL / min, a liquefied carbon dioxide gas flow rate of 20 mL / min, a treatment pressure of 20 Mpa, a dissolution bath temperature of 20 ° C., and a reaction coil holding unit temperature of 40 ° C. were passed through and extracted for 3 hours.
Next, water was added to the obtained supercritical extract to prepare an ethanol concentration of 5% by mass or less. The supernatant was removed from the resulting precipitate by decantation to obtain a precipitate. The obtained precipitate was dissolved by adding 2 L of ethanol, and the resulting solution was cooled to 5 ° C. The insoluble matter produced by cooling was clarified and filtered, and water was added to the obtained filtrate to prepare an ethanol concentration of 5% by mass or less. The resulting precipitate was decanted and the supernatant was removed, and the precipitate was dried under reduced pressure to obtain 1.2 kg of Ponkan supercritical extract. The content of nobiletin, which is an active ingredient in the Ponkan supercritical extract, was 45% by mass.
About the obtained Ponkan supercritical extract, the residual pesticide was measured by GC-MS in the same manner as in Example 1. As a result, no methidathion was detected and the pesticide was removed. In addition, it was confirmed that the content of nobiletin, which is an active ingredient, was not changed by the supercritical treatment.

  According to the method for removing residual agricultural chemicals from plant extracts of the present invention, residual agricultural chemicals can be efficiently removed from plant extracted materials, quality deterioration can be prevented, continuous extraction processing is possible, and a significant cost reduction is achieved. it can. The plant extract obtained by the method for removing residual pesticides of the plant extract of the present invention has no loss or deterioration of plant extract components, almost all of the residual pesticides are removed, and is excellent in safety, food additives, cosmetics. It can be widely used in various fields such as ingredients, pharmaceuticals, and quasi drugs.

FIG. 1 is a schematic view showing an example of a microbubble supercritical processing apparatus of the present invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Stock solution supply tank 2 High pressure pump 3 Liquid carbon dioxide cylinder 4 Cooler 5 Carbon dioxide supply pump 6 Heater 7 Dissolution tank 8 Reaction coil (holding part)
9 Mesh Filter 10 Gas-Liquid Separation Tank 11 Gas-Liquid Separation Sensor 12 Separation Tank 13 Trap 16 Processed Sample Tank 20 Decompression Unit

Claims (5)

  A carbon dioxide gas dissolving step in which the plant extract material is brought into contact with a carbon dioxide fluid to dissolve the carbon dioxide gas fluid in the plant extract material, and the plant extract material in which the carbon dioxide gas is dissolved is converted into a supercritical to subcritical state of carbon dioxide gas. And a carbon dioxide gas supercritical treatment step in which the plant extract material is held and stirred, and a carbon dioxide gas removal step in which the plant extract material is rapidly depressurized to normal pressure to remove carbon dioxide from the plant extract material. A method for removing residual pesticides from plant extracts.   The method for removing residual pesticides from plant extracts according to claim 1, wherein in the carbon dioxide dissolving step, carbon dioxide fluid that is microbubbled through a mesh filter having a mesh of 100 µm or less is used.   A plant extract material is obtained by extracting a plant extract raw material with water, a hydrophilic solvent and a mixed solvent thereof, and a plant extract obtained by extracting the plant extract with water, a hydrophilic solvent and a mixed solvent thereof. The method for removing residual agricultural chemicals from plant extracts according to any one of claims 1 to 2, wherein the solution is any one of plant extract solutions dissolved in any of the above.   A plant extract obtained by extracting a plant extract material with water, ethanol, or a mixed solvent thereof, and a plant extract obtained by dissolving a plant extract with water, ethanol, or a mixed solvent thereof. The method for removing a residual pesticide from a plant extract according to claim 3, wherein the method is any one of solutions. A plant extract obtained by the method for removing residual agricultural chemicals according to any one of claims 1 to 4.

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