CN112843115A - Method for removing benzopyrene in folium artemisiae argyi alcohol extract - Google Patents
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Abstract
The invention discloses a method for removing benzopyrene in an folium artemisiae argyi alcohol extract, which aims to solve the problems that the prior art only considers the removal effect of a removing agent on the benzopyrene, and the relative loss of the removing agent on effective components is difficult to control, so that the economic benefit is considered to be deficient, and a method for removing the benzopyrene by aiming at a plant extract is not available; the method comprises the following steps: crushing and sieving folium Artemisiae Argyi, adding folium Artemisiae Argyi into extraction tank, adding food grade ethanol, cold soaking or heating for 1-5 times, filtering the extractive solution to obtain filtrate I, and then adding nanometer TiO2-siliconFiltering the filtrate again with a filter made of the diatomite composite material to obtain a filtrate II, and finally concentrating the filtrate II to obtain the folium artemisiae argyi extract. The method not only reduces the content of benzopyrene to 0.5ppb which is far higher than the Korean KFDA standard, has high safety, but also has high yield of the prepared folium artemisiae argyi extract, no obvious loss of index components, low removal cost, economy and effectiveness.
Description
Technical Field
The invention belongs to the technical field of plant component extraction, and particularly relates to a method for removing benzopyrene in an folium artemisiae argyi alcohol extract.
Background
The folium artemisiae argyi has rich medicinal sources, low price and easy obtainment, and simultaneously has broad spectrum and low toxicity, so that various developed formulations of the folium artemisiae argyi are widely applied to medicines, health care products, foods and cosmetics, the folium artemisiae argyi extract is applied to various traditional and modern formulations including pills, powder, decoction, externally-applied paste, moxibustion agents, fumigation agents, sachets, vinum and the like, and the new formulation relates to injections, tablets, capsules, aerosols, mixtures, granules, teas, enemas, various compound preparations and patches, beta-cyclodextrin inclusion, dropping pills and the like; the daily chemical products are applied to 10 types of products such as essential oil, medicine pillow, mosquito-repellent incense, toothpaste, face cleaning cream, Aitonkang, shampoo, shower gel, disinfectant and the like, and other products comprise mugwort leaf mosquito-repellent incense, mugwort leaf insecticide and the like. At present, a series of cosmetic products such as a mugwort massage cream, a mugwort shower gel, a mugwort moisturizing lotion and the like are developed in korea by taking mugwort as a main raw material; and Japan also makes fragrant deinsectization pillow from Chinese mass imported folium Artemisiae Argyi. In the aspect of food additives, the folium artemisiae argyi extract is used as a health food additive in Japan for processing weight-losing food, and further comprises folium artemisiae argyi health product preparations, health waistbands, snake-moxa sanitary napkins and the like; in addition, Korean KFDA has a very high demand for the extract of Artemisia princeps, and the most critical technical requirement is that the benzopyrene content is less than 20 ppb.
Benzopyrene is originally separated from coal tar, and mainly comes from waste gas generated by incomplete combustion of fuels such as coal, petroleum and natural gas in industrial production and living processes, and fat, cholesterol, protein, carbohydrate and the like generated under high-temperature conditions in the smoking, baking and frying processes of food. The presence of benzopyrene has a great threat to human health, and is a representative of strong carcinogenic substances, which can cause DNA damage after invading human body and possibly induce canceration. The benzopyrene in the folium artemisiae argyi mainly comes from the processing process, and the folium artemisiae argyi extract which is not subjected to removal process treatment cannot meet the requirement of 20 ppb.
At present, more technical means are provided for removing benzopyrene from oily liquid, and a certain idea is disclosed in some documents, for example, chinese patent application with publication number CN104958321A discloses an application of egg yolk oil and egg oil with benzopyrene removed in preparation of drugs for treating allergic rhinitis, wherein activated carbon is used for removing benzopyrene from the egg oil; also, for example, chinese patent application publication No. CN102432583A discloses a method for preparing d- α tocopherol acetate with high purity of low benzopyrene, which comprises preparing d- α tocopherol acetate with high purity of low benzopyrene by using a remover (one or a mixture of two or more of activated carbon and silica gel); also, for example, the chinese patent application with publication No. CN107008226A discloses a process for removing aflatoxin and benzopyrene from peanut oil, which uses a special adsorbent to remove benzopyrene from peanut oil; also, for example, the chinese patent application with publication No. CN101381154A discloses a method for advanced treatment of benzopyrene in drinking water source by using biofilm, which selects specific genetically engineered bacteria biofilm to treat benzopyrene in drinking water; also, for example, chinese patent application publication No. CN102640805A discloses a method for deodorizing, deacidifying, and removing benzopyrene from edible vegetable oil, which uses a molecular distillation apparatus to remove benzopyrene from edible vegetable oil; also, for example, chinese patent application publication No. CN107805544A discloses a method for removing benzopyrene from edible vegetable oil, which comprises removing benzopyrene from edible vegetable oil by using a mixed adsorbent prepared from diatomite, hydrochloric acid, sodium dodecyl sulfate, kaolinite and sepiolite; also, for example, the chinese patent application publication No. CN104108783A discloses a method for rapidly, efficiently and selectively degrading trace amounts of benzopyrene in water, which removes trace amounts of benzopyrene in water through an ozone catalytic oxidation reactor; as another example, the Chinese patent application with publication No. CN109470790A discloses a method for synchronously measuring benzopyrene in soil by rapid solvent extraction and purification, which adopts solvent extraction method to purify benzopyrene in soilPyrene; also, for example, the Chinese patent application with publication No. CN102260591A discloses a method for removing benzopyrene in edible oil by TiO2-treating the edible oil with a ZnO composite nanomaterial to remove benzopyrene; also, for example, chinese patent application publication No. CN107057848A discloses a process for removing benzopyrene from oil, which uses a special DNA aqueous solution to remove benzopyrene from edible oil; also, for example, chinese patent application publication No. CN105013799A discloses a method for degrading benzopyrene/lead pollution in road dust by irradiation, which even removes benzopyrene in road dust by irradiation (ultraviolet photochemical degradation); the benzopyrene is removed by adopting various methods in the technology, but most of the benzopyrene is directed at animal and vegetable oil and water, and the influence on the functional components of the original removed substances is not considered.
In addition, the publication number CNCN107348327A also discloses a method for removing benzopyrene from solid natural phytosterol, which is a crude product of natural phytosterol, after a polar organic solvent (one or two of methanol, isopropanol and ethanol) is dissolved, a removing agent (one or any proportion of porous activated carbon, silica gel, activated clay and a molecular sieve is added for mixing), benzopyrene in the crude product of solid natural phytosterol is directly removed, the content of benzopyrene in the obtained solid natural phytosterol is stably less than 1ppb by detection, and the requirements of European and American food-grade certification are met. The invention can obtain better effect, but the application range is very narrow, and is only limited to the removal of benzopyrene in natural phytosterol, and the patent only considers the removal effect of the removal agent on the benzopyrene, does not verify the relative loss of the removal agent on effective components, and has poor economic benefit.
In addition, publication No. CN107550965 also discloses a preparation method of a folium artemisiae argyi extract, which is obtained by coarsely crushing folium artemisiae argyi, sieving, extracting with 95% ethanol, filtering, concentrating, adsorbing with activated carbon, and concentrating, and has the advantages of high yield, high content of eupatilin and jaceosidin as active ingredients, low content of carcinogen benzopyrene, low pesticide residue, high product safety, simple process, easy operation, and suitability for industrial production. However, the invention uses more active carbon for adsorption, so that the active ingredients of eupatilin and jaceosidin are simultaneously adsorbed and lost, and the transfer rate of the active ingredients is not described by the technology.
At present, methods for removing benzopyrene from plant extracts are reported, but in the prior removal technology, the content of benzopyrene in folium artemisiae argyi alcohol extracts reaches the requirement of 0.5ppb, and the loss of effective components of folium artemisiae argyi is not obvious, which is basically difficult to realize in the field, so that in order to meet related requirements, the removal method for removing benzopyrene from plant extracts needs to be improved urgently.
Disclosure of Invention
(1) Technical problem to be solved
Aiming at the defects of the prior art, the invention aims to provide a method for removing benzopyrene in an folium artemisiae argyi alcohol extract, which aims to solve the problems that the prior art only considers the removal effect of a remover on the benzopyrene and is difficult to control the relative loss of the remover on effective components, so that the economic benefit is considered to be deficient, and a method special for removing the benzopyrene from a plant extract is not available; the method not only reduces the content of benzopyrene to 0.5ppb which is far higher than the Korean KFDA standard, has high safety, but also has high yield of the prepared folium artemisiae argyi extract, no obvious loss of index components, low removal cost, economy and effectiveness.
(2) Technical scheme
In order to solve the technical problem, the invention provides a method for removing benzopyrene in an folium artemisiae argyi alcohol extract, which comprises the following specific steps: crushing and sieving folium artemisiae argyi medicinal materials, controlling the aperture of a sieve to be less than 0.4cm, adding the crushed medicinal materials into an extraction tank, adding food-grade ethanol, controlling the mass percentage concentration of the ethanol to be 30-97%, controlling the adding mass of the ethanol to be 6-30 times of the mass of the crushed and sieved folium artemisiae argyi medicinal materials, performing cold soaking or heating extraction for 1-5 times, filtering an extracting solution to obtain a filtrate I, controlling a filtering filter cloth to be 100 meshes and 300 meshes, and then filling nano TiO into the filtrate I2Filtering the filtrate again by using a filter made of the diatomite composite material to obtain a filtrate II, and finally concentrating the filtrate II to obtain a paste, namely the folium artemisiae argyi extract.
Preferably, after the extracting solution is filtered to obtain a first filtrate, the first filtrate passes through 400 meshes and 5um filter bags respectively, then is subjected to reduced pressure concentration through a single-effect external circulation concentrator, the vacuum degree of the reduced pressure concentration is controlled to be-0.05 MPa to-0.10 MPa, the temperature is controlled to be 50-70 ℃, the reduced pressure concentration is carried out until the relative ratio is 0.62-0.65, so as to obtain a feed liquid, and then the feed liquid is filled with nano TiO2And (4) filtering the obtained feed liquid again by using a filter made of the diatomite composite material to obtain filtrate II.
Preferably, the solution is filled with nano TiO2And in the process of filtering the filtrate again by using the filter made of the diatomite composite material, controlling the flow rate of the filtrate I to be 400L/h, and filtering the filtrate I by using a 1um filter to obtain filtrate II.
Preferably, the second filtrate is concentrated by adding the second filtrate into a spherical concentrator for vacuum concentration, the vacuum degree of the vacuum concentration is controlled to be-0.05 MPa to-0.10 MPa, the temperature is controlled to be 50 ℃ to 70 ℃, and the vacuum concentration is carried out until the relative density is 1.24.
Preferably, the nano TiO2The diatomite composite material is nano TiO2And diatomite as raw material, and preparing the supported TiO by a mechanical force activation method in a mechanical grinding system of an aqueous medium2-a diatomite composite material.
Further, the mechanical grinding system is used for carrying out superfine stirring grinding, the grinding parameters are 1000r/min, grinding medium balls adopt 3 diameters, the ratio of phi 3mm to phi 2mm to phi 1mm is 5: 3: 2, the ball-material ratio is 3: 1, and diatomite and nano TiO are mixed according to the proportion2Is 40: 60, and adding nano TiO2Triethanolamine with the mass fraction of 1 percent is used as a dispersant, and is mixed and ground on a superfine stirring mill for 80min to obtain TiO2-a diatomite composite material.
(3) Advantageous effects
Compared with the prior art, the invention has the beneficial effects that: the process of the invention is carried out by TiO2The diatomite composite material removes benzopyrene in the folium artemisiae argyi alcohol extract, so that the content of the benzopyrene is reduced to 0.5ppb which is far higher than the Korean KFDA standard, the safety is high, the prepared folium artemisiae argyi extract has high yield,the content of active ingredients of eupatilin and jaceosidin is high, and the transfer rate exceeds 80 percent; meanwhile, the influence of the removing agent on index components is considered, so that the method has no obvious loss, low removing cost, economy and effectiveness; in addition, the method is suitable for industrial production, and the process is simple and easy to operate.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood and obvious, the technical solutions in the embodiments of the present invention are clearly and completely described below to further illustrate the invention, and obviously, the described embodiments are only a part of the embodiments of the present invention, but not all the embodiments.
Example 1
The specific embodiment is a method for extracting a folium artemisiae argyi extract without benzopyrene, which comprises the following specific steps:
1) extraction: taking 1000kg of folium artemisiae argyi medicinal material, crushing the folium artemisiae argyi medicinal material, sieving the folium artemisiae argyi medicinal material by using a sieve with the aperture of 0.4cm, adding the crushed medicinal material into 20000L of 90% ethanol solution by mass percentage, heating and refluxing for extraction for 3 times, filtering the extracting solution by using a 100-mesh filter bag to obtain a first filtrate, and putting the first filtrate into a storage tank for later use.
2) Concentration: respectively filtering the filtrate I with 400 meshes and 5um filter bags, carrying out reduced pressure concentration by a single-effect external circulation concentrator, controlling the vacuum degree of the reduced pressure concentration to be-0.05 MPa to-0.10 MPa, controlling the temperature to be 55-65 ℃, carrying out reduced pressure concentration until the relative ratio is 0.62-0.65, and recovering the solvent to obtain the feed liquid.
3) And (3) filtering: the feed liquid is filled with nano TiO2And filtering again by using a filter made of the diatomite composite material, controlling the flow rate of the feed liquid to be 400L/h, and filtering by using a 1um filter to obtain a filtrate II.
4) Concentration: and adding the filtrate II into a spherical concentrator for vacuum concentration, controlling the vacuum degree of the vacuum concentration to be between-0.05 and-0.10 MPa, controlling the temperature to be between 60 and 70 ℃, concentrating under reduced pressure until the relative density is 1.24, and flowing into a hundred thousand grade clean area through a pipeline to obtain a paste, namely the folium artemisiae argyi extract.
The nano TiO2The filter made of the diatomite composite material is the TiO2The diatomite composite material is prepared by filling the filler in a conical cylinder body serving as a container by a wet method. The conical cylinder body is made of 304 stainless steel, the diameter of the round bottom of the conical cylinder body is 60cm, the height of the conical cylinder body is 120cm, 5 independent chambers are formed in the cylinder body in a partition mode through 4 layers of stainless steel partition plates, the height of each layer of chamber is about 20cm, and each layer of partition plate comprises a plurality of round holes with the aperture of 0.4 mm. The bottom of the cylinder body is a stainless steel bottom cover with a detachable hoop structure, and the cylinder body can be opened when filling and discharging; the cylinder body is arranged on the bracket and can be turned over up and down to facilitate filling, the cylinder body is turned over to the bottom upwards during filling, the bottom cover is opened, and nano TiO is filled2Suspending liquid of the diatomite composite material to a scale, covering a stainless steel clapboard paved with qualitative filter paper, and then continuously filling nano TiO in sequence2Covering the diatomite composite material with the partition plate until the 5 chambers are filled with the conforming material, and fastening the bottom cover to obtain the nano TiO2-a diatomite composite filter. Compared with the traditional filter, the filter increases the contact area of the feed liquid and the filter paper, forms multi-stage filtration, and improves the filtering effect and efficiency while playing a multi-stage removal role for benzo-pyrene.
Wherein the nano TiO2The diatomite composite material is prepared by taking nano titanium dioxide and diatomite as raw materials and adopting a mechanical force activation method to prepare supported TiO in a mechanical grinding system of an aqueous medium2A diatomite composite material. The superfine stirring mill in mechanical grinding system has operating parameters of 1000r/min rotation speed, 3 kinds of grinding medium balls in the ratio of phi 3mm to phi 2mm to phi 1mm of 5 to 3 to 2 and ball material ratio of 3 to 1. By mixing diatomite and nano TiO2(40: 60), adding nano TiO2Triethanolamine with the mass fraction of 1 percent is used as a dispersant, and is mixed and ground on a superfine stirring mill for 80min to obtain TiO2A diatomite composite material.
In addition, by detecting the folium artemisiae argyi extract prepared in the embodiment, the content of the carcinogen benzopyrene is 0.4ppb, the yield is 10.3%, and other related data are as follows:
example 2
The specific embodiment is a method for extracting a folium artemisiae argyi extract without benzopyrene, which comprises the following specific steps:
1) extraction: taking 1000kg of folium artemisiae argyi medicinal material, crushing the folium artemisiae argyi medicinal material, sieving the folium artemisiae argyi medicinal material by using a sieve with the aperture of 0.35cm, adding the crushed medicinal material into 20000L of 30% ethanol solution by mass percentage, carrying out cold-leaching reflux extraction for 5 times, filtering an extracting solution by using a 200-mesh filter bag to obtain a first filtrate, and putting the first filtrate into a storage tank for later use.
2) Concentration: respectively filtering the filtrate I with 400 meshes and 5um filter bags, carrying out reduced pressure concentration by a single-effect external circulation concentrator, controlling the vacuum degree of the reduced pressure concentration to be-0.05 MPa to-0.10 MPa, controlling the temperature to be 60-70 ℃, carrying out reduced pressure concentration until the relative ratio is 0.62-0.65, and recovering the solvent to obtain the feed liquid.
3) And (3) filtering: the feed liquid is filled with nano TiO2And filtering again by using a filter made of the diatomite composite material, controlling the flow rate of the feed liquid to be 400L/h, and filtering by using a 1um filter to obtain a filtrate II.
4) Concentration: and adding the filtrate II into a spherical concentrator for vacuum concentration, controlling the vacuum degree of the vacuum concentration to be between-0.05 and-0.10 MPa, controlling the temperature to be between 50 and 60 ℃, concentrating under reduced pressure until the relative density is 1.24, and flowing into a hundred thousand grade clean area through a pipeline to obtain a paste, namely the folium artemisiae argyi extract.
The nano TiO2The filter made of the diatomite composite material is the TiO2The diatomite composite material is prepared by filling the filler in a conical cylinder body serving as a container by a wet method. The conical cylinder body is made of 304 stainless steel, the diameter of the round bottom of the conical cylinder body is 60cm, the height of the conical cylinder body is 120cm, 5 independent chambers are formed in the cylinder body in a partition mode through 4 layers of stainless steel partition plates, the height of each layer of chamber is about 20cm, and each layer of partition plate comprises a plurality of round holes with the aperture of 0.4 mm. The bottom of the cylinder body is a stainless steel bottom cover with a detachable hoop structure, and the cylinder body can be opened when filling and discharging; the cylinder body is arranged on the bracket and can be turned over up and down, so that the filling is convenient, the cylinder body is turned over to the bottom upwards during the filling, the bottom cover is opened, and the filling container is arrangedTiO rice2Suspending liquid of the diatomite composite material to a scale, covering a stainless steel clapboard paved with qualitative filter paper, and then continuously filling nano TiO in sequence2Covering the diatomite composite material with the partition plate until the 5 chambers are filled with the conforming material, and fastening the bottom cover to obtain the nano TiO2-a diatomite composite filter. Compared with the traditional filter, the filter increases the contact area of the feed liquid and the filter paper, forms multi-stage filtration, and improves the filtering effect and efficiency while playing a multi-stage removal role for benzo-pyrene.
Wherein the nano TiO2The diatomite composite material is prepared by taking nano titanium dioxide and diatomite as raw materials and adopting a mechanical force activation method to prepare supported TiO in a mechanical grinding system of an aqueous medium2A diatomite composite material. The superfine stirring mill in mechanical grinding system has operating parameters of 1000r/min rotation speed, 3 kinds of grinding medium balls in the ratio of phi 3mm to phi 2mm to phi 1mm of 5 to 3 to 2 and ball material ratio of 3 to 1. By mixing diatomite and nano TiO2(40: 60), adding nano TiO2Triethanolamine with the mass fraction of 1 percent is used as a dispersant, and is mixed and ground on a superfine stirring mill for 80min to obtain TiO2A diatomite composite material.
In addition, by detecting the folium artemisiae argyi extract prepared in the embodiment, the content of the carcinogen benzopyrene is 0.38ppb, the yield is 10.1%, and other related data are as follows:
example 3
The specific embodiment is a method for extracting a folium artemisiae argyi extract without benzopyrene, which comprises the following specific steps:
1) extraction: taking 1000kg of folium artemisiae argyi medicinal material, crushing the folium artemisiae argyi medicinal material, sieving the folium artemisiae argyi medicinal material by using a sieve with the aperture of 0.4cm, adding the crushed medicinal material into 20000L of 97% ethanol solution in percentage concentration by mass, heating, refluxing and extracting for 1 time, filtering the extracting solution by using a 300-mesh filter bag to obtain a first filtrate, and putting the first filtrate into a storage tank for later use.
2) And (3) filtering: the filtrate I is filled with nano TiO2And filtering again by using a filter made of the diatomite composite material, controlling the flow rate of the feed liquid to be 400L/h, and filtering by using a 1um filter to obtain a filtrate II.
3) Concentration: and adding the filtrate II into a spherical concentrator for vacuum concentration, controlling the vacuum degree of the vacuum concentration to be between-0.05 and-0.10 MPa, controlling the temperature to be between 50 and 65 ℃, concentrating under reduced pressure until the relative density is 1.24, and flowing into a hundred thousand grade clean area through a pipeline to obtain a paste, namely the folium artemisiae argyi extract.
The nano TiO2The filter made of the diatomite composite material is the TiO2The diatomite composite material is prepared by filling the filler in a conical cylinder body serving as a container by a wet method. The conical cylinder body is made of 304 stainless steel, the diameter of the round bottom of the conical cylinder body is 60cm, the height of the conical cylinder body is 120cm, 5 independent chambers are formed in the cylinder body in a partition mode through 4 layers of stainless steel partition plates, the height of each layer of chamber is about 20cm, and each layer of partition plate comprises a plurality of round holes with the aperture of 0.4 mm. The bottom of the cylinder body is a stainless steel bottom cover with a detachable hoop structure, and the cylinder body can be opened when filling and discharging; the cylinder body is arranged on the bracket and can be turned over up and down to facilitate filling, the cylinder body is turned over to the bottom upwards during filling, the bottom cover is opened, and nano TiO is filled2Suspending liquid of the diatomite composite material to a scale, covering a stainless steel clapboard paved with qualitative filter paper, and then continuously filling nano TiO in sequence2Covering the diatomite composite material with the partition plate until the 5 chambers are filled with the conforming material, and fastening the bottom cover to obtain the nano TiO2-a diatomite composite filter. Compared with the traditional filter, the filter increases the contact area of the feed liquid and the filter paper, forms multi-stage filtration, and improves the filtering effect and efficiency while playing a multi-stage removal role for benzo-pyrene.
Wherein the nano TiO2The diatomite composite material is prepared by taking nano titanium dioxide and diatomite as raw materials and adopting a mechanical force activation method to prepare supported TiO in a mechanical grinding system of an aqueous medium2A diatomite composite material. The superfine stirring mill in the mechanical grinding system has the operating parameters of 1000r/min rotation speed and 3 kinds of grinding medium balls of different diametersThe ratio of phi 3mm to phi 2mm to phi 1mm is 5: 3: 2, and the ratio of the ball material to the material is 3: 1. By mixing diatomite and nano TiO2(40: 60), adding nano TiO2Triethanolamine with the mass fraction of 1 percent is used as a dispersant, and is mixed and ground on a superfine stirring mill for 80min to obtain TiO2A diatomite composite material.
In addition, by detecting the folium artemisiae argyi extract prepared in the embodiment, the content of the carcinogen benzopyrene is 0.45ppb, the yield is 10.4%, and other related data are as follows:
the method of the technical proposal adopts TiO2The diatomite composite material removes benzopyrene in the folium artemisiae argyi alcohol extract, so that the content of the benzopyrene is reduced to 0.5ppb which is far higher than the Korean KFDA standard, the safety is high, the prepared folium artemisiae argyi extract has high yield, the contents of active components eupatilin and jaceosidin are high, and the transfer rate exceeds 80 percent; meanwhile, the influence of the removing agent on index components is considered, so that the method has no obvious loss, low removing cost and economy and effectiveness.
Having thus described the principal technical features and basic principles of the invention, and the advantages associated therewith, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description is described in terms of various embodiments, not every embodiment includes only a single embodiment, and such descriptions are provided for clarity only, and those skilled in the art will recognize that the embodiments described herein can be combined as a whole to form other embodiments as would be understood by those skilled in the art.
Claims (6)
1. A method for removing benzopyrene in folium artemisiae argyi alcohol extract is characterized by comprising the following specific steps: crushing and sieving folium artemisiae argyi medicinal materials, controlling the aperture of a sieve to be less than 0.4cm, adding the crushed medicinal materials into an extraction tank, adding food-grade ethanol, controlling the mass percentage concentration of the ethanol to be 30-97%, controlling the adding mass of the ethanol to be 6-30 times of the mass of the crushed and sieved folium artemisiae argyi medicinal materials, performing cold soaking or heating extraction for 1-5 times, filtering an extracting solution to obtain a filtrate I, controlling a filtering filter cloth to be 100 meshes and 300 meshes, and then filling nano TiO into the filtrate I2Filtering the filtrate again by using a filter made of the diatomite composite material to obtain a filtrate II, and finally concentrating the filtrate II to obtain a paste, namely the folium artemisiae argyi extract.
2. The method for removing benzopyrene in folium artemisiae argyi alcohol extract according to claim 1, wherein after filtering the extracting solution to obtain a first filtrate, the first filtrate is respectively filtered through 400-mesh and 5-um filter bags, then the first filtrate is subjected to reduced pressure concentration through a single-effect external circulation concentrator, the vacuum degree of the reduced pressure concentration is controlled to be-0.05 MPa to-0.10 MPa, the temperature is controlled to be 50-70 ℃, the reduced pressure concentration is carried out until the relative ratio is 0.62-0.65, so as to obtain a feed liquid, and then the feed liquid is filled with nano TiO2And (4) filtering the obtained feed liquid again by using a filter made of the diatomite composite material to obtain filtrate II.
3. The method for removing benzopyrene in folium artemisiae argyi alcohol extract according to claim 1, wherein the folium artemisiae argyi alcohol extract is filled with nano TiO2And in the process of filtering the filtrate again by using the filter made of the diatomite composite material, controlling the flow rate of the filtrate I to be 400L/h, and filtering the filtrate I by using a 1um filter to obtain filtrate II.
4. The method for removing benzopyrene in the folium artemisiae argyi alcohol extract according to claim 1, wherein the second filtrate is concentrated by adding the second filtrate into a spherical concentrator for vacuum concentration, the vacuum degree of the vacuum concentration is controlled to be-0.05 MPa to-0.10 MPa, the temperature is controlled to be 50-70 ℃, and the vacuum concentration is carried out until the relative density is 1.24.
5. The method for removing benzopyrene in folium artemisiae argyi alcohol extract according to claim 1, wherein the nano TiO is2The diatomite composite material is nano TiO2And diatomite as raw material, and preparing the supported TiO by a mechanical force activation method in a mechanical grinding system of an aqueous medium2-a diatomite composite material.
6. The method for removing benzopyrene in the alcohol extract of artemisia argyi as claimed in claim 5, wherein the mechanical grinding system is used for superfine stirring and grinding, the grinding speed is 1000r/min, the grinding media balls have 3 diameters, the ratio of phi 3mm to phi 2mm to phi 1mm is 5: 3: 2, the ball-material ratio is 3: 1, and diatomite and nano TiO are mixed according to the ratio of phi 3mm to phi 2mm, and the ball-material ratio is 3: 12Is 40: 60, and adding nano TiO2Triethanolamine with the mass fraction of 1 percent is used as a dispersant, and is mixed and ground on a superfine stirring mill for 80min to obtain TiO2-a diatomite composite material.
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| CN114053752A (en) * | 2021-11-18 | 2022-02-18 | 西安天一生物技术股份有限公司 | Method for removing benzopyrene in hypericum perforatum extract by using solvent |
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