CN109157867B - Method for quickly eliminating pesticide residues in ginseng extract - Google Patents
Method for quickly eliminating pesticide residues in ginseng extract Download PDFInfo
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Abstract
The invention provides a method for eliminating pesticide residues in a ginseng extracting solution, and belongs to the field of pesticide residue elimination and medicinal component purification. The invention utilizes the polarity difference between the residual pesticide and the ginsenoside, the residual pesticide with lower polarity is absorbed by CNFs/CFs, and the ginsenoside with higher polarity is retained in the ginseng extract. The whole extraction process is convenient and simple to operate, the time is short, and the aims of eliminating residual pesticide and retaining ginsenoside can be achieved. And only a few solvents need to be introduced, the environment is friendly, and large-scale industrial elimination can be realized by establishing a large-scale pesticide residue elimination device. The elimination method of the invention has elimination rates of 94.6%, 97.4%, 92.8% and 96.3% for PCNB (pentachloronitrobenzene), HCH (hexachlorocyclohexane), Procymidone (Procymidone) and DDT (bis-p-chlorophenyl trichloroethane) in the ginseng extract respectively, and the retention rate of ginsenoside reaches more than 88%.
Description
Technical Field
The invention relates to the technical field of pesticide residue elimination and medicinal component purification, in particular to a method for quickly eliminating pesticide residues in a ginseng extract.
Background
Ginseng, one of the three treasures of northeast China, is regarded as the king of Baicao, and has the effects of regulating the balance of excitation process and inhibition process of central nervous system, preventing and treating acute and chronic altitude diseases caused by anoxia, resisting fatigue, improving body adaptability, etc. However, during the cultivation of ginseng, the pesticide residue in the ginseng extract can be caused by the problems of pesticide residue in soil, blind pesticide spraying of part of ginseng farmers and the like. And after long-term contact or eating of food containing pesticide residues, the pesticide can be continuously accumulated in the body, which has potential threat to human health, namely chronic poisoning, which can affect the nervous system, destroy the liver function, cause physiological disorder, affect the reproductive system, generate abnormal fetus and cause various problems such as cancer and the like. Therefore, it is very necessary to eliminate the residual pesticide in the ginseng extract.
Currently, the commonly used methods for eliminating pesticide residues mainly include dispersion liquid-liquid microextraction, liquid-phase microextraction, solid-phase extraction, solid-phase microextraction and the like, and the methods generally have the defects of use of a large amount of organic solvents, long analysis time, more experimental steps, complex operation and the like, for example, CN 106267897a discloses a method for quickly separating ginsenoside and residual pesticide in ginseng, wherein carbon fibers and activated carbon fibers are used as a two-dimensional system, and pesticide residues are eliminated through four elution processes.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for rapidly eliminating pesticide residues in a ginseng extract. The invention takes carbon nano fiber/carbon fiber as a material, adsorbs residual pesticide by utilizing a similar compatibility principle, quickly eliminates the residual pesticide and retains ginsenoside.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for rapidly eliminating pesticide residues in a ginseng extract comprises the following steps:
providing a ginseng extract;
providing a carbon nanofiber/carbon fiber material;
and mixing the ginseng extract and the carbon nano fiber/carbon fiber material to adsorb the residual pesticide, and removing the residual pesticide in the ginseng extract.
Preferably, the ginseng extract is prepared by the following steps: extracting ginseng and its leaves and stems with an extractant comprising water.
Preferably, the extractant further comprises ethanol, and the volume fraction of the ethanol in the extractant is 0-25%.
Preferably, the mass ratio of pesticide residues in the ginseng extract to the carbon nanofiber/carbon fiber extraction material is 1: 30-150.
Preferably, the mixing is performed under vortexing conditions.
Preferably, the frequency of the vortex oscillation is 50-60 Hz.
Preferably, the mixing comprises the steps of:
filling the carbon nanofiber/carbon fiber extraction material in a filter membrane form to obtain a filter membrane;
and (3) passing the ginseng extracting solution through the filter membrane.
Preferably, when the concentration of pesticide residues in the ginseng extract is 0.5 mug/mL, the passing rate of the ginseng extract is not more than 1 mL/min.
Preferably, the mixing comprises the steps of:
filling the carbon nanofiber/carbon fiber extraction material in a packed column to obtain a packed column;
and (3) passing the ginseng extract through the packed column.
Preferably, the packing density of the packed column is 0.024g/cm when the concentration of pesticide residue in the ginseng extract is 0.5 μ g/mL2The passing time is not less than 10 min.
The invention provides a method for quickly eliminating pesticide residues in a ginseng extract, which comprises the following steps: providing a ginseng extract; providing a carbon nanofiber/carbon fiber (CNFs/CFs) material; and mixing the ginseng extract and the carbon nano fiber/carbon fiber material to adsorb the residual pesticide, and removing the residual pesticide in the ginseng extract. The invention establishes an on-line elimination method, which utilizes the polarity difference between the residual pesticide and the ginsenoside, the residual pesticide with lower polarity is absorbed by CNFs/CFs, and the ginsenoside with higher polarity is retained in the ginseng extract. The whole extraction process is convenient and simple to operate, the time is short, and the aims of eliminating residual pesticide and retaining ginsenoside can be achieved. And the method only needs to introduce less solvent, is environment-friendly, and realizes large-scale industrial elimination of enterprises by establishing a large-scale pesticide residue eliminating device. The data of the embodiment shows that the elimination method provided by the invention has elimination rates of 94.6%, 97.4%, 92.8% and 96.3% for PCNB (pentachloronitrobenzene), HCH (hexachlorocyclohexane), Procymidone (Procymidone) and DDT (bis-p-chlorophenyl trichloroethane) in the ginseng extract respectively, the ginsenoside is retained, and the retention rate of the ginsenoside is more than 88%.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a flow chart of vortex oscillation of the ginseng extract and carbon nanofiber/carbon fiber material according to the present invention;
FIG. 2 is a schematic view showing a process of passing the ginseng extract solution through a filtration membrane according to the present invention;
FIG. 3 is a schematic view showing the flow of the ginseng extract solution of the present invention through a packed column.
Detailed Description
The invention provides a method for quickly eliminating pesticide residues in a ginseng extract, which comprises the following steps:
providing a ginseng extract;
providing a carbon nanofiber/carbon fiber material;
and mixing the ginseng extract and the carbon nano fiber/carbon fiber material to adsorb the residual pesticide, and removing the residual pesticide in the ginseng extract.
The invention provides a ginseng extract. In the present invention, the ginseng extract is preferably prepared by a method comprising the steps of: extracting ginseng and its leaves and stems with an extractant comprising water.
In the invention, the extractant preferably further comprises ethanol, and the volume fraction of the ethanol in the extractant is preferably 0-25%.
In the present invention, the pesticide residue in the ginseng extract preferably includes PCNB (pentachloronitrobenzene), HCH (hexachlorocyclohexane), Procymidone (Procymidone), and DDT (bis-p-chlorophenyl trichloroethane). In the present invention, the concentration of the pesticide residue in the ginseng extract is preferably 500ng/mL, and the concentration of the ginsenoside in the ginseng extract is preferably 5. mu.g/mL.
The present invention does not specifically limit the specific way of extraction, and may adopt the extraction method known to those skilled in the art.
The source of the ginseng is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
The present invention provides carbon nanofiber/carbon fiber materials (CNFs/CFs). The source of the carbon nanofiber/carbon fiber material is not particularly limited, and the carbon nanofiber/carbon fiber material can be prepared by the preparation method disclosed in CN201610681314.1 or by the following preparation method:
(1) removing slurry: first, 10 bundles of 6.0cm pure Carbon Fibers (CFs) (3000 in 1 bundle) after desizing were taken out from the dryer, and the obtained bundle was calcined in a muffle furnace at 450 ℃ for 30min and then subjected to Soxhlet extraction with acetone for 12 hours to remove the size.
(2) Acid treatment of the carbon fiber surface: and (3) treating the dried carbon fiber with nitric acid/sulfuric acid/phosphoric acid solution with the volume ratio of 1:3:9 for 1.5h at normal temperature and pressure, (carrying out ultrasonic treatment for 0.5h, and soaking for 1h) to ensure that the surface of the carbon fiber is rich in carboxyl, so that the carbon fiber is easy to modify in the next step. Repeatedly leaching acidified carbon fibers (CFs-H) with ultrapure water until the surface is neutral, and drying in an oven.
(3) Deposition of catalyst on the carbon fiber surface acidified carbon fibers were immersed in a prepared catalyst solution (surfactant (P123, Pluronic P123, EO20PO70EO20, Mav ═ 5800), ethanol, hydrochloric acid, H2O: ethyl orthosilicate: nickel nitrate 0.0103:21.4:0.04:9.36:1:0.47) for 12 h.
(4) And washing the carbon fibers with a catalyst solution until the carbon fibers are dispersed, and then carrying out suction filtration.
(5) And (3) calcining the carbon fiber obtained in the fourth step in a tubular muffle furnace at 450 ℃ for 30 min.
(6) Preparing CNFs/CFs composite fiber by chemical vapor deposition, namely placing carbon fiber with a catalyst uniformly coated on the surface of CFs-H in a tube furnace, and introducing 150-300 cc/min at the heating rate of 2-20 ℃/min-1Heating inert gas (nitrogen, argon or helium) at a flow rate to 500-700 ℃, and introducing 10-50 cc min-1H of (A) to (B)230min, reducing the catalyst, and then introducing a carbon source C2H2Gas for 30min (10-60 cc min)-1) After the chemical vapor deposition reaction is finished, H is turned off2And C2H2And cooling to room temperature.
In the invention, the mass ratio of pesticide residues to the carbon nano fibers/carbon fiber materials in the ginseng extract is preferably 1: 30-150, and more preferably 1: 50-150.
In the present invention, the mixing is preferably carried out under vortex oscillation conditions.
In the invention, the frequency of the vortex oscillation is preferably 50-60 Hz, and the time of the vortex oscillation is not less than 1 min.
Fig. 1 is a flow chart of vortex oscillation of a ginseng extract and a carbon nanofiber/carbon fiber material, wherein after adsorption is completed in fig. 1, after removing residual pesticide in the ginseng extract, the adsorbed carbon nanofiber/carbon fiber material is separated and then immersed in Dichloromethane (DCM), ultrasonic desorption is performed for 1min, and liquid obtained by ultrasonic desorption is subjected to nitrogen-blowing concentration, volume fixing, water removal (anhydrous sodium sulfate), filtration (aperture is 0.45 μm) in sequence, and pesticide residue is analyzed by gas chromatography-mass spectrometry; filtering the adsorbed Ginseng radix extractive solution with water phase filter membrane (pore diameter of 0.45 μm), and analyzing ginsenoside residue by liquid chromatography-mass spectrometry.
In the present invention, the mixing preferably comprises the steps of:
filling the carbon nanofiber/carbon fiber material in a filter membrane form to obtain a filter membrane;
and (3) filtering the ginseng extract by using a filter membrane.
In the present invention, when the concentration of the residual pesticide in the ginseng extract is 0.5. mu.g/mL, the passing rate of the ginseng extract is preferably not more than 1 mL/min.
FIG. 2 is a schematic view showing the flow of the ginseng extract through the filtration membrane according to the present invention, wherein the ginseng extract is separated from the residual pesticide by passing through the filtration membrane.
In the present invention, the mixing preferably comprises the steps of:
filling the carbon nanofiber/carbon fiber material in a packed column to obtain a packed column;
and (3) passing the ginseng extract through the packed column.
In the present invention, when the packing density of the packed column is 0.024g/cm2When the time is not less than 10min, the passing time is preferably not less than 10 min.
Fig. 3 is a schematic flow diagram of the ginseng extract liquid passing through the packed column, and in fig. 3, the liquid flow is controlled by the control valve, so that the ginseng extract liquid passes through the packed column to realize the separation of ginsenoside and residual pesticide.
The method for rapidly eliminating pesticide residues in the ginseng extract according to the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Preparation of carbon nanofiber/carbon fiber materials (CNFs/CFs)
(1) Removing slurry: first, 10 bundles of 6.0cm pure Carbon Fibers (CFs) (3000 in 1 bundle) after desizing were taken out from the dryer, and the obtained bundle was calcined in a muffle furnace at 450 ℃ for 30min and then subjected to Soxhlet extraction with acetone for 12 hours to remove the size.
(2) Acid treatment of the carbon fiber surface: and (3) treating the dried carbon fiber with nitric acid/sulfuric acid/phosphoric acid solution with the volume ratio of 1:3:9 for 1.5h at normal temperature and pressure, (carrying out ultrasonic treatment for 0.5h, and soaking for 1h) to ensure that the surface of the carbon fiber is rich in carboxyl, so that the carbon fiber is easy to modify in the next step. Repeatedly leaching acidified carbon fibers (CFs-H) with ultrapure water until the surface is neutral, and drying in an oven.
(3) Deposition of catalyst on the carbon fiber surface acidified carbon fibers were immersed in a prepared catalyst solution (surfactant (P123, Pluronic P123, EO20PO70EO20, Mav ═ 5800), ethanol, hydrochloric acid, H2O: ethyl orthosilicate: nickel nitrate 0.0103:21.4:0.04:9.36:1:0.47) for 12 h.
(4) And washing the carbon fibers with a catalyst solution until the carbon fibers are dispersed, and then carrying out suction filtration.
(5) And (3) calcining the carbon fiber obtained in the fourth step in a tubular muffle furnace at 450 ℃ for 30 min.
(6) Preparing CNFs/CFs composite fiber by chemical vapor deposition, namely placing carbon fiber with catalyst uniformly coated on the surface of CFs-H in a tubular furnace, and introducing 150cc & min at the heating rate of 20 ℃/min-1Heating to 500 deg.C with inert gas (nitrogen) at flow rate, and introducing 1cc min-1H of (A) to (B)230min, reducing the catalyst, and then introducing a carbon source C2H2Gas 30min (10cc min)-1) After the chemical vapor deposition reaction is finished, H is turned off2And C2H2And cooling to room temperature to obtain CNFs/CFs.
Extracting Ginseng radix and folium Ginseng and stem with water to obtain Ginseng radix extractive solution, wherein the concentration of residual pesticide in Ginseng radix extractive solution is 500ng/mL, the concentration of ginsenoside is 5 μ g/mL, and the pesticide residue comprises PCNB (pentachloronitrobenzene), HCH (hexachlorocyclohexane), Procymidone (Procymidone) and DDT (bis-p-chlorophenyl trichloroethane).
Filling the large-scale device with CNFs/CFs, wherein the amount of the filling depends on the concentration of the residual pesticide in the ginseng extract, the mass ratio of the pesticide residue to the CNFs/CFs is 150:1, namely 150g of CNFs/CFs can eliminate 1g of pesticide residue in absolute amount, and the density is 0.024g/cm2The filtering time is 10 min;
and (3) enabling a certain volume of the ginseng extract to pass through a packed column at a constant speed, and removing pesticide residues in the ginseng extract.
Example 2
Same as example 1, except that 10% C was used2H5OH-H2And O, preparing the ginseng extracting solution.
Example 3
Same as example 1, except that 25% C was used2H5OH-H2And O, preparing the ginseng extracting solution.
Table 1 shows the results of the detection of the elimination rate of pesticide residues in examples 1 to 3 of the present invention, and Table 2 shows the results of the detection of the residue rate of ginsenosides in examples 1 to 3 of the present invention, and from tables 1 to 2, an on-line microextraction method is established, in which the residual pesticide with smaller polarity is adsorbed by CNFs/CFs, and the ginsenoside with larger polarity is retained in the ginseng extract, by utilizing the polarity difference between the residual pesticide and the ginsenoside. The whole extraction process is convenient and simple to operate, the time is short, and the aims of eliminating residual pesticide and retaining ginsenoside can be achieved. And the method only needs to introduce less solvent, is environment-friendly, and can realize large-scale industrial elimination by establishing a large-scale pesticide residue elimination device.
Table 1 examples 1 to 3 results of detection of pesticide residue removal rate (%) (n is 3)
Table 2 examples 1 to 3 results of determination of ginsenoside remaining ratio (%) (n is 3)
Rb1, Rc, Rb2, Re, Rd, Rg1 and Rf in Table 2 are names of seven ginsenoside.
Table 3 shows the results of the test of the pesticide residue removal (%) in the mass ratio of different pesticide residues to CNFs/CFs
Example 4
The procedure for preparing carbon nanofiber/carbon fiber materials (CNFs/CFs) and ginseng extract was the same as in example 1, the CNFs/CFs were filled in the form of a filter membrane, the residual pesticide in the ginseng extract was eliminated on the filter membrane by the filtration, the ginsenoside remained in the ginseng extract, as shown in fig. 2, and the test results are shown in table 4.
TABLE 4 pesticide residue removal (%) test results (n ═ 3)
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for rapidly eliminating pesticide residues in a ginseng extract comprises the following steps:
providing a ginseng extract; the ginseng extracting solution is prepared by the method comprising the following steps: extracting ginseng and leaves and stems of ginseng with an extractant, wherein the extractant comprises water and ethanol, and the volume fraction of the ethanol in the extractant is 10%;
providing a carbon nanofiber/carbon fiber material; the preparation method of the carbon nanofiber/carbon fiber material comprises the following steps:
(1) removing slurry: firstly, taking 10 bundles of 6.0cm pure carbon fibers after pulp removal from a dryer, putting 1 bundle of 3000 pure carbon fibers in a muffle furnace, calcining for 30min at 450 ℃, and then performing Soxhlet extraction for 12h by using acetone to remove pulp;
(2) acid treatment of the carbon fiber surface: treating the dried carbon fiber with nitric acid/sulfuric acid/phosphoric acid solution with a volume ratio of 1:3:9 at normal temperature and pressure for 1.5h, specifically performing ultrasonic treatment for 0.5h, soaking for 1h to ensure that the surface of the carbon fiber is rich in carboxyl, repeatedly leaching the acidified carbon fiber with ultrapure water until the surface is neutral, and drying in an oven;
(3) depositing a catalyst on the surface of the carbon fiber, namely soaking the acidified carbon fiber in the prepared catalyst solution for 12 hours; surfactant in the catalyst solution: ethanol: hydrochloric acid: h2O: ethyl orthosilicate: the mass ratio of the nickel nitrate is 0.0103:21.4:0.04:9.36:1:0.47, and the surfactant is P123, Pluronic P123, EO20PO70EO20，Mav＝5800；
(4) Washing the carbon fibers with a catalyst solution until the carbon fibers are dispersed, and then performing suction filtration;
(5) calcining the carbon fiber obtained in the step (4) in a tubular muffle furnace at 450 ℃ for 30 min;
(6) preparing CNFs/CFs composite fiber by chemical vapor deposition, namely putting carbon fiber with a catalyst uniformly coated on the surface of acidified carbon fiber in a tube furnace, and introducing 150-300 cc/min at the heating rate of 2-20 ℃/min-1Heating inert gas at a flow rate to 500-700 ℃, and introducing 10-50 cc/min-1H of (A) to (B)230min, reducing the catalyst, and then introducing a carbon source C2H2Gas deposition for 30minAfter the end of the reaction, H is switched off2And C2H2Cooling to room temperature, wherein the inert gas is nitrogen, argon or helium, and C2H2The flow rate of the gas is 10 to 60 cc/min-1；
Mixing the ginseng extract and the carbon nanofiber/carbon fiber material to adsorb pesticide residues, and removing the pesticide residues in the ginseng extract; when the concentration of the residual pesticide in the ginseng extracting solution is 0.5 mug/mL, the passing speed of the ginseng extracting solution is not more than 1 mL/min.
2. The elimination method according to claim 1, wherein the mass ratio of the pesticide residue to the carbon nanofiber/carbon fiber material in the ginseng extract is 1:30 to 150.
3. The abatement method of claim 1, wherein the mixing is performed under vortexing conditions.
4. The cancellation method according to claim 1, characterized in that said mixing comprises the steps of:
filling the carbon nanofiber/carbon fiber material in a filter membrane form to obtain a filter membrane;
and (3) passing the ginseng extracting solution through the filter membrane.
5. The elimination method according to claim 4, wherein when the concentration of pesticide residues in the ginseng extract is 0.5 μ g/mL, the passing rate of the ginseng extract is not more than 1 mL/min.
6. The cancellation method according to claim 1, characterized in that said mixing comprises the steps of:
filling the carbon nanofiber/carbon fiber material in a packed column to obtain a packed column;
and (3) passing the ginseng extract through the packed column.
7. The elimination method according to claim 6, wherein the packed column has a packing density of 0.024g/cm when the concentration of the pesticide residue in the ginseng extract solution is 0.5 μ g/mL2The passing time is not less than 10 min.
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| JP2006078419A (en) * | 2004-09-13 | 2006-03-23 | Sumika Technoservice Kk | Analytical method and analytical system for pesticide |
| CN102128901A (en) * | 2010-12-20 | 2011-07-20 | 天津市农业科学院中心实验室 | Method for processing ginseng sample containing sulfonylurea pesticide residue before measurement |
| CN105784855A (en) * | 2014-12-24 | 2016-07-20 | 中国科学院兰州化学物理研究所 | Application of carbon nanotube-grafted carbon fiber composite filiform filler in vaporizing chamber of gas chromatograph |
| CN106267897A (en) * | 2016-09-26 | 2017-01-04 | 延边大学 | Ginsenoside and the method for residual pesticide in sharp separation Radix Ginseng |
| CN106353439A (en) * | 2016-08-17 | 2017-01-25 | 延边大学 | Method and device for preparing carbon nano-fiber/carbon fiber solid-phase micro-extraction coatings |
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| JP2006078419A (en) * | 2004-09-13 | 2006-03-23 | Sumika Technoservice Kk | Analytical method and analytical system for pesticide |
| CN102128901A (en) * | 2010-12-20 | 2011-07-20 | 天津市农业科学院中心实验室 | Method for processing ginseng sample containing sulfonylurea pesticide residue before measurement |
| CN105784855A (en) * | 2014-12-24 | 2016-07-20 | 中国科学院兰州化学物理研究所 | Application of carbon nanotube-grafted carbon fiber composite filiform filler in vaporizing chamber of gas chromatograph |
| CN106353439A (en) * | 2016-08-17 | 2017-01-25 | 延边大学 | Method and device for preparing carbon nano-fiber/carbon fiber solid-phase micro-extraction coatings |
| CN106267897A (en) * | 2016-09-26 | 2017-01-04 | 延边大学 | Ginsenoside and the method for residual pesticide in sharp separation Radix Ginseng |
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