CN114773358B - Method for extracting rotenone from radix Puerariae - Google Patents
Method for extracting rotenone from radix Puerariae Download PDFInfo
- Publication number
- CN114773358B CN114773358B CN202210349569.3A CN202210349569A CN114773358B CN 114773358 B CN114773358 B CN 114773358B CN 202210349569 A CN202210349569 A CN 202210349569A CN 114773358 B CN114773358 B CN 114773358B
- Authority
- CN
- China
- Prior art keywords
- ethanol
- rotenone
- water
- solution
- resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229940080817 rotenone Drugs 0.000 title claims abstract description 63
- JUVIOZPCNVVQFO-UHFFFAOYSA-N rotenone Natural products O1C2=C3CC(C(C)=C)OC3=CC=C2C(=O)C2C1COC1=C2C=C(OC)C(OC)=C1 JUVIOZPCNVVQFO-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000011347 resin Substances 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 54
- 238000005406 washing Methods 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 21
- 239000012065 filter cake Substances 0.000 claims description 20
- 238000002791 soaking Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 244000046146 Pueraria lobata Species 0.000 claims description 2
- 235000010575 Pueraria lobata Nutrition 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims 3
- 238000000605 extraction Methods 0.000 abstract description 23
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 7
- 239000003480 eluent Substances 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 231100000614 poison Toxicity 0.000 abstract description 3
- 239000003440 toxic substance Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000004809 thin layer chromatography Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000002390 rotary evaporation Methods 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 235000019890 Amylum Nutrition 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 241001124076 Aphididae Species 0.000 description 1
- 241000220485 Fabaceae Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000255969 Pieris brassicae Species 0.000 description 1
- 241000500437 Plutella xylostella Species 0.000 description 1
- 241000353135 Psenopsis anomala Species 0.000 description 1
- 241000750718 Pterocarpus santalinus Species 0.000 description 1
- 241000700141 Rotifera Species 0.000 description 1
- 241000913745 Spatholobus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/14—Ortho-condensed systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to the technical field of plant extraction, and provides a method for extracting rotenone from radix puerariae lobatae, which can realize the maximum extraction of the rotenone from the radix puerariae lobatae Ge Shezhong by selecting an ethanol water solution as an extracting solution, save the ethanol consumption, simultaneously avoid a part of other organic matters in Sha Geshe from entering the extracting solution, and reduce the later-stage separation difficulty; because the rotenone has smaller polarity and poorer water solubility, the adsorption of the rotenone in the extract is realized by utilizing the characteristics of high adsorption speed and large adsorption capacity of organic matters with poor water solubility and larger resistance to the diffusion from the water phase to the resin because the surface of the inner hole of the weak-polarity macroporous adsorption resin is provided with weak-polarity groups; the water-soluble impurities adsorbed on the resin are eluted by water, and finally the rotenone is eluted by ethanol. The reagent used by the extracting solution and the eluent adopted by the invention is only ethanol and water, so that the use of benzene and toluene which are high toxic substances is avoided, and the environmental protection of the rotenone extraction method is improved.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to a method for extracting rotenone from radix puerariae lobatae.
Background
Rotenone is an organic substance, molecular formula C 23 H 22 O 6 Is a substance with strong specificity in toxicology, and has strong contact killing and stomach poisoning effects on insects, especially cabbage butterfly larvae, plutella xylostella and aphids.
Since rotenone is present in roots of plants of genus rotifer of family Leguminosae produced in tropical and subtropical areas of asia, it is also contained in some herbs such as ground melon seeds, pterocarpus santalinus, and spatholobus stem roots, and is thus obtained by means of plant extraction in the prior art. The extraction method mainly comprises the following steps: oscillation extraction, microwave extraction, supercritical CO 2 Extraction, etc., but the solvents commonly used in the above methods are toluene or benzene, and the above solvents are generally carcinogenic.
Therefore, it is highly desirable to provide a more environmentally friendly rotenone extraction method.
Disclosure of Invention
In view of the above, the invention aims to provide a method for extracting rotenone from radix puerariae lobatae, the reagents used in the extraction method provided by the invention are ethanol and water, the use of cancerogenic reagents benzene and toluene is avoided, and the method is environment-friendly.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for extracting rotenone from radix puerariae lobatae, which comprises the following steps:
(1) Sha Geshe is soaked in ethanol water solution to obtain impregnating solution;
(2) Removing ethanol in the impregnating solution obtained in the step (1) to obtain an aqueous solution to be extracted;
(3) Carrying out chromatography on the aqueous solution to be extracted obtained in the step (2) by adopting weak-polarity macroporous adsorption resin to obtain rotenone;
the chromatographic reagent in the step (3) is water and ethanol in sequence.
Preferably, the radix Puerariae Lobatae in step (1) is powder.
Preferably, the particle size of the powder is 40-70 mesh.
Preferably, the particle size of the powder is 50 to 60 mesh.
Preferably, the mass content of the ethanol in the ethanol aqueous solution in the step (1) is 40-60%.
Preferably, the mass content of ethanol in the ethanol aqueous solution in the step (1) is 50%.
Preferably, the mass of the sand-arrowroot leaves in the step (1) and the volume ratio of the ethanol water solution are (10-60) g:1L.
Preferably, the soaking time in the step (1) is 60-80 h.
Preferably, the soaking time in the step (1) is 65-75 hours.
Preferably, the weak polar macroporous resin in the step (3) comprises AB-8 macroporous adsorption resin, XDA-6 macroporous adsorption resin or XDA-1B macroporous adsorption resin.
The invention provides a method for extracting rotenone from radix puerariae lobatae, which comprises the following steps: firstly, putting Sha Geshe into an ethanol water solution for soaking to obtain an impregnating solution; then removing ethanol in the obtained impregnating solution to obtain an aqueous solution of the to-be-extracted substance; and finally, carrying out chromatography on the obtained aqueous solution of the extract to be extracted by adopting weak-polarity macroporous adsorption resin to obtain the rotenone. According to the invention, the ethanol water solution is selected as the extracting solution, so that the maximum extraction of the sand Ge Shezhong rotenone can be realized, the ethanol consumption is saved, meanwhile, a part of other organic matters in Sha Geshe are prevented from entering the extracting solution, and the later-stage separation difficulty is reduced; because the rotenone has smaller polarity and poorer water solubility, the adsorption of the rotenone in the extract is realized by utilizing the characteristics of high adsorption speed and large adsorption capacity of organic matters with poor water solubility and larger resistance to the diffusion from the water phase to the resin because the surface of the inner hole of the weak-polarity macroporous adsorption resin is provided with weak-polarity groups; the water-soluble impurities adsorbed on the resin are eluted by water, and finally the rotenone is eluted by ethanol. The reagent used by the extracting solution and the eluent adopted by the invention is only ethanol and water, so that the use of benzene and toluene which are high toxic substances is avoided, and the environmental protection of the rotenone extraction method is improved.
Drawings
FIG. 1 is a liquid chromatogram of rotenone extracted in example 1 of the present invention;
FIG. 2 is a mass spectrum of rotenone extracted in example 1 of the present invention.
Detailed Description
The invention provides a method for extracting rotenone from radix puerariae lobatae, which comprises the following steps:
(1) Sha Geshe is soaked in ethanol water solution to obtain impregnating solution;
(2) Removing ethanol in the impregnating solution obtained in the step (1) to obtain an aqueous solution to be extracted;
(3) Carrying out chromatography on the aqueous solution to be extracted obtained in the step (2) by adopting weak-polarity macroporous adsorption resin to obtain rotenone;
the chromatographic reagent in the step (3) is water and ethanol in sequence.
Sha Geshe is placed in ethanol water solution for soaking, so as to obtain the impregnating solution.
The source of Sha Geshe is not particularly limited, and the leaf part of the natural-grown radix puerariae can be selected. Since the leaves of the root of Amylum Puerariae Radicis contain much rotenone, the present invention uses the leaves of Amylum Puerariae Radicis as the extraction target.
In the present invention, the Sha Geshe is preferably a powder. In the present invention, the particle size of the powder is preferably 40 to 70 mesh, more preferably 50 to 60 mesh. The invention limits the granularity of the powder to the above range, can well realize the full extraction of rotenone, and simultaneously avoids the excessively small granularity, and fine impurities are difficult to filter in the later filtering process.
According to the invention, sha Geshe is preferably subjected to drying, crushing, grinding and sieving in sequence to obtain powder.
The drying method is not particularly limited, and the drying method known to those skilled in the art may be used to sufficiently remove the water in Sha Geshe.
The crushing operation is not particularly limited in the present invention, and a crushing method well known to those skilled in the art is adopted to crush Sha Geshe having a relatively large volume into a smaller volume.
The grinding mode is not particularly limited in the present invention, and Sha Geshe may be ground to a desired particle size by grinding modes well known to those skilled in the art.
The method of sieving is not particularly limited, and powder with larger particle size can be removed by sieving method well known to those skilled in the art to obtain powder with required particle size.
In the present invention, the mass content of ethanol in the aqueous ethanol solution is preferably 40 to 60%, more preferably 50%. The method selects the ethanol water solution with the concentration as the impregnating solution, can realize the maximum extraction of the sand Ge Shezhong rotenone, saves the ethanol consumption, simultaneously avoids a part of other organic matters in Sha Geshe from entering the extracting solution, and reduces the later-stage separation difficulty.
In the present invention, the mass ratio of Sha Geshe to the volume ratio of the aqueous ethanol solution is preferably (10 to 60) g:1L, more preferably (15 to 55) g:1L. The Sha Geshe and ethanol aqueous solution dosage is controlled in the range, so that the rotenone can be extracted to the greatest extent, and waste caused by excessive ethanol aqueous solution is avoided.
In the present invention, the soaking time is preferably 60 to 80 hours, more preferably 65 to 75 hours. The invention limits the soaking time to the above range, and can realize the maximum extraction of rotenone.
The operation of the soaking is not particularly limited in the invention, and a soaking mode well known to those skilled in the art is adopted to submerge the solid phase in the liquid phase.
After the soaking is finished, the invention preferably filters the soaked system to obtain filtrate and filter cake.
The filtering mode is not particularly limited, and the solid-liquid separation can be realized by adopting a filtering mode well known to a person skilled in the art.
After the filter cake is obtained, the filter cake is preferably washed to obtain a washing liquid.
In the present invention, the solvent for washing is preferably the same as the aqueous ethanol solution used for soaking. The invention washes the filter cake, avoids partial rotenone from remaining on the filter cake, and reduces the extraction efficiency.
The method for washing the filter cake is not particularly limited, and the rotenone remaining in the filter cake is washed out by adopting a washing method well known to a person skilled in the art.
After the filtrate and the washing solution are obtained, the filtrate and the washing solution are preferably combined to obtain the impregnating solution.
After the immersion liquid is obtained, the invention removes the ethanol in the immersion liquid to obtain the water solution of the to-be-extracted matter.
The method of removing ethanol is not particularly limited, and a solvent removal method well known to those skilled in the art may be employed. In the embodiment of the invention, the removing mode is preferably rotary steaming. In the invention, the boiling points of the ethanol and the water are different, so that the ethanol is removed firstly in the rotary evaporation process, the recovery of the ethanol is realized, and the influence of the ethanol in the later separation is reduced.
Because solid impurities are separated out from the solution after the ethanol is removed, the invention preferably filters the system after the ethanol is removed to obtain filtrate and filter cake containing the to-be-extracted substance; then washing the obtained filter cake to obtain a washing liquid; and combining the filtrate with the washing solution to obtain an aqueous solution of the to-be-extracted substance. In the present invention, the reagent used for the washing is preferably water. The invention adopts water for washing, and avoids reintroducing ethanol into the ethanol-removing solution system.
After the aqueous solution to be extracted is obtained, the invention adopts weak-polarity macroporous adsorption resin to carry out chromatography on the aqueous solution to be extracted to obtain rotenone.
In the present invention, the weakly polar macroporous resin preferably comprises an AB-8 macroporous adsorption resin, an XDA-6 macroporous adsorption resin or an XDA-1B macroporous adsorption resin, more preferably an AB-8 macroporous adsorption resin. The invention utilizes the characteristic that the weak polar macroporous adsorption resin has weak polar groups on the surface of the inner holes, and has high adsorption speed and large adsorption capacity for organic matters with poor water solubility and large resin phase resistance when the organic matters are diffused from the water phase to the resin phase resistance, thereby realizing the adsorption of rotenone in the extract. The weak-polarity macroporous adsorption resin is a common commercial product, wherein the AB-8 macroporous adsorption resin has higher specific surface area and better separation effect on rotenone.
In the invention, the chromatographic reagent is water and ethanol in sequence. The invention does not have special regulation on the dosage of the water, and the water-soluble impurities in the extract are fully removed. The invention has no special standard for the dosage of the ethanol, and can realize the full elution of the rotenone in the extract. The determination criteria for the adequate removal of the water-soluble impurities and the adequate elution of rotenone are not particularly specified in the present invention, and the determination criteria for whether or not a specific substance is present in a solution well known to those skilled in the art may be employed. Such as liquid chromatography or TLC thin layer chromatography silica gel plates. In an embodiment of the present invention, the determination is preferably a TLC thin layer chromatography silica gel plate. The invention uses developing agent to develop the collected chromatography liquid on TLC thin layer chromatography silica gel plate, to judge whether the water of the chromatography liquid has water-soluble impurity, when there is almost no water-soluble impurity, it is changed into ethanol to elute until the rotenone is eluted completely. In the present invention, the developing agent is preferably petroleum ether and ethyl acetate; the volume ratio of petroleum ether to ethyl acetate is preferably 25:1.
after chromatography is completed, the ethanol eluent after chromatography is preferably subjected to solvent removal and drying in sequence to obtain rotenone.
The solvent removal method is not particularly limited in the present invention, and the solvent in the solution is removed by the solvent removal method well known to those skilled in the art, and the solute is retained.
The drying method is not particularly limited, and the solvent remaining in the solute may be further removed by drying methods well known to those skilled in the art.
The invention provides a method for extracting rotenone from radix puerariae lobatae, which can realize the maximum extraction of the rotenone from the radix puerariae lobatae by selecting ethanol water solution as an extracting solution, save the ethanol consumption, simultaneously avoid a part of other organic matters in Sha Geshe from entering the extracting solution, and reduce the later separation difficulty; because the rotenone has smaller polarity and poorer water solubility, the adsorption of the rotenone in the extract is realized by utilizing the characteristics of high adsorption speed and large adsorption capacity of organic matters with poor water solubility and larger resistance to the diffusion from the water phase to the resin because the surface of the inner hole of the weak-polarity macroporous adsorption resin is provided with weak-polarity groups; the water-soluble impurities adsorbed on the resin are eluted by water, and finally the rotenone is eluted by ethanol. The reagent used by the extracting solution and the eluent adopted by the invention is only ethanol and water, so that the use of benzene and toluene which are high toxic substances is avoided, and the environmental protection of the rotenone extraction method is improved.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Sha Geshe is dried for 24 hours, crushed and ground into powder, and screened with 60 meshes; weighing 500g of powder, pouring the powder into a container, adding 20L of 50% ethanol aqueous solution, stirring and soaking for 72h, filtering, washing a filter cake with the 50% ethanol aqueous solution for three times, combining the washing solution and the filtrate, performing rotary evaporation for 10h together to recover ethanol, filtering the solution in a rotary spherical digester, washing the obtained filter cake with water, combining the filter cake with the filtrate to obtain an aqueous solution to be extracted, pouring the aqueous solution to be extracted into a column filled with AB-8 macroporous adsorption resin, washing with deionized water for three times, slowly eluting with ethanol to obtain a rotenone solution, removing ethanol, and drying to obtain the rotenone.
Example 2
Sha Geshe is dried for 24 hours, crushed and ground into powder, and screened with a 50 mesh screen; weighing 100g of powder, pouring the powder into a container, adding 5L of 50% ethanol water solution, stirring and soaking for 48h, filtering, washing a filter cake with the 50% ethanol water solution for three times, combining the washing solution and the filtrate, performing rotary evaporation for 3h together to recover ethanol, filtering the solution in a rotary spherical digester, washing the obtained filter cake with water, combining the filter cake with the filtrate to obtain an aqueous solution to be extracted, pouring the aqueous solution to be extracted into a column filled with AB-8 macroporous adsorption resin, washing with deionized water for three times, slowly eluting with ethanol to obtain a rotenone solution, removing ethanol, and drying to obtain the rotenone.
Example 3
Sha Geshe is dried for 24 hours, crushed and ground into powder, and screened with a 50 mesh screen; weighing 50g of powder, pouring the powder into a container, adding 10L of 50% ethanol water solution, stirring and soaking for 24 hours, filtering, washing a filter cake with the 50% ethanol water solution for three times, combining the washing solution and the filtrate, performing rotary evaporation for 1 hour together to recover ethanol, filtering the solution in a rotary spherical digester, washing the obtained filter cake with water, combining the filter cake with the filtrate to obtain an aqueous solution to be extracted, pouring the aqueous solution to be extracted into a column filled with AB-8 macroporous adsorption resin, washing with deionized water for three times, slowly eluting with ethanol to obtain a rotenone solution, removing ethanol, and drying to obtain the rotenone.
The maximum absorption peak at 12 minutes (the peak position of rotenone in the prior art is about 12 minutes) can be seen in the liquid chromatogram of fig. 1 by detecting the sand Ge Shecu extract obtained in example 1 by liquid chromatography; from the mass spectrum of fig. 2, it can be seen that the maximum molecular weight is 395.14 (rotenone standard molecular weight 394.42); in summary, the peak position and the maximum molecular weight of the maximum peak in the extract are almost equivalent to those of rotenone in the prior art, and the main component of the extract can be judged to be rotenone.
The extraction effect of rotenone of examples 1-3 was tested, and the test results are shown in Table 1.
TABLE 1 extraction Effect of rotenone from examples 1 to 3
| Sha Geshe weight of powder (g) | Rotenone content in Pueraria lobata | Total weight of extract (g) | Content of rotenone in the extract | Extraction efficiency | |
| Example 1 | 500 | 0.1015％ | 0.654 | 57.89％ | 74.6％ |
| Example 2 | 100 | 0.1015％ | 0.133 | 60.21％ | 78.9％ |
| Example 3 | 50 | 0.1012％ | 0.059 | 69.73％ | 81.3％ |
As can be seen from Table 1, the extraction method provided by the invention can also extract rotenone with higher content under the condition of almost no toxic solvent.
While only the preferred embodiments of the present invention have been described, it should be noted that those skilled in the art could make several improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be considered as the protection scope of the present invention.
Claims (4)
1. A method for extracting rotenone from radix Puerariae comprises the following steps:
(1) Soaking Sha Geshe in ethanol water solution; filtering the soaked system to obtain filtrate and filter cake; washing the filter cake to obtain a washing liquid; combining the filtrate and the washing liquid to obtain an impregnating liquid;
(2) Removing ethanol in the impregnating solution obtained in the step (1) to obtain an aqueous solution to be extracted;
(3) Carrying out chromatography on the aqueous solution to be extracted obtained in the step (2) by adopting weak-polarity macroporous adsorption resin to obtain rotenone;
the chromatographic reagent in the step (3) is water and ethanol in sequence;
the radix puerariae lobatae leaves in the step (1) are powder;
the granularity of the powder is 50-60 meshes;
the mass content of the ethanol in the ethanol water solution in the step (1) is 40-60%;
the soaking time in the step (1) is 65-75 hours.
2. The method according to claim 1, wherein the mass content of ethanol in the aqueous ethanol solution in step (1) is 50%.
3. The method according to claim 1, wherein the ratio of the mass of the kudzuvine leaf to the volume of the ethanol aqueous solution in the step (1) is (10-60) g:1L.
4. The method of claim 1, wherein the weakly polar macroporous resin in step (3) comprises an AB-8 macroporous adsorbent resin, an XDA-6 macroporous adsorbent resin, or an XDA-1B macroporous adsorbent resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210349569.3A CN114773358B (en) | 2022-04-02 | 2022-04-02 | Method for extracting rotenone from radix Puerariae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210349569.3A CN114773358B (en) | 2022-04-02 | 2022-04-02 | Method for extracting rotenone from radix Puerariae |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114773358A CN114773358A (en) | 2022-07-22 |
| CN114773358B true CN114773358B (en) | 2024-01-09 |
Family
ID=82426701
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210349569.3A Active CN114773358B (en) | 2022-04-02 | 2022-04-02 | Method for extracting rotenone from radix Puerariae |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114773358B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB559647A (en) * | 1942-07-17 | 1944-02-29 | Stafford Allen And Sons Ltd | Improvements in the manufacture of rotenone |
| CN101619062A (en) * | 2009-07-02 | 2010-01-06 | 华宝食用香精香料（上海）有限公司 | Natural fibrauretine crystal and macroporous adsorbent resin preparation method thereof |
| CN104381321A (en) * | 2014-11-03 | 2015-03-04 | 山东省农业科学院植物保护研究所 | Plant source biological composition and preparation method thereof as well as application of plant source biological composition to prevention and treatment of green onion maggots |
| CN110903297A (en) * | 2019-12-20 | 2020-03-24 | 海南省林业科学研究所 | Macroporous resin extraction method of rotenone and analogue |
-
2022
- 2022-04-02 CN CN202210349569.3A patent/CN114773358B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB559647A (en) * | 1942-07-17 | 1944-02-29 | Stafford Allen And Sons Ltd | Improvements in the manufacture of rotenone |
| CN101619062A (en) * | 2009-07-02 | 2010-01-06 | 华宝食用香精香料（上海）有限公司 | Natural fibrauretine crystal and macroporous adsorbent resin preparation method thereof |
| CN104381321A (en) * | 2014-11-03 | 2015-03-04 | 山东省农业科学院植物保护研究所 | Plant source biological composition and preparation method thereof as well as application of plant source biological composition to prevention and treatment of green onion maggots |
| CN110903297A (en) * | 2019-12-20 | 2020-03-24 | 海南省林业科学研究所 | Macroporous resin extraction method of rotenone and analogue |
Non-Patent Citations (1)
| Title |
|---|
| 运用乙醇渗漉法优化三叶鱼藤中鱼藤酮提取工艺—基于响应面法;郭霞等;《华中师范大学学报（自然科学版）》;第54卷(第1期);第60-64段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114773358A (en) | 2022-07-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106831353B (en) | Method for extracting cannabidiol from cannabis sativa | |
| Feng et al. | Removal of lead, zinc and cadmium from contaminated soils with two plant extracts: Mechanism and potential risks | |
| CA2317495A1 (en) | A process for the isolation, recovery and purification of non-polar extractives | |
| CN104610410A (en) | Extraction process of ginseng saponin Rd | |
| CN102631414B (en) | SepHaniadelavayi Diels total alkaloid extraction and purification technology | |
| CN104147093A (en) | Method for rapidly extracting licorice flavonoids at room temperature | |
| Gallardo et al. | Biosorption of rare-earth elements from aqueous solutions using walnut shell | |
| CN114773358B (en) | Method for extracting rotenone from radix Puerariae | |
| CN105566414A (en) | Method for separating and purifying four flavone glycosides from waxberry pulp | |
| CN102266378A (en) | Method for developing and utilizing overground and underground parts of astragalus comprehensively | |
| CN107652166B (en) | Separation method of mangnolia officinalis bisphenol | |
| Inoue et al. | Adsorptive removal of uranium and thorium with a crosslinked persimmon peel gel. | |
| CN109884199B (en) | Method for measuring content of flavonoid components in honey | |
| US6132726A (en) | Process for removing impurities from natural product extracts | |
| CN104189073B (en) | The preparation method of salvianolic acid | |
| JPH1067771A (en) | Production of catechins having low catechin content | |
| Saha et al. | Factors affecting the extraction of dieldrin-14C from soil | |
| CN114181227A (en) | Method for extracting physalin and method for purifying extracting solution thereof | |
| King | Gas chromatographic determination of diquat residues in potato tubers | |
| CN106336440A (en) | Method for extracting and separating out oleanolic acid from olive leaves | |
| CN1284504A (en) | Methof of extracting isoflavone, saponin, oligosaccharide and protein simultaneously from defatted soybean dregs | |
| CN105477029A (en) | Preparation method of evening primrose seed flavone | |
| CN112588272B (en) | Flavonoid substance adsorbent and preparation method thereof | |
| CN110003143A (en) | A method of extracting natural Japanese yew alcohol | |
| CN114057826B (en) | Preparation method of reference substance of toosendanin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |