CN101455708B - Method for benzo (alpha) pyrene removal from red clover extract using ultramicro communication technique - Google Patents
Method for benzo (alpha) pyrene removal from red clover extract using ultramicro communication technique Download PDFInfo
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Abstract
The invention discloses a method for eliminating benzo[a] pyrene in red clover extract by ultrafine grinding technology. The method has steps of crushing the red clover extract into granules having grain diameter no more than 75 um by ultrafine grinding, stirring the grinded extract by solvent of acetic ester and petroleum ether having equivalent mass ratio, extracting by hot reflux, drying, and thereby the product is obtained. The invention obviously improves elimination rate for benzo[a] pyrene in red clover extract.
Description
Technical field
The invention belongs to the Chinese medicine extraction applied technical field, be specifically related to the method that a kind of using ultramicro communication technique removes benzo in the Herba Trifolii Pratentis extract [a] pyrene.
Background technology
Benzo [a] pyrene claims 3 again, the 4-benzopyrene.It is a kind of polycyclic aromatic hydrocarbon that is made of 5 phenyl ring, and molecular formula is C
20H
12, molecular weight is 252.Structural formula is as shown below.
Benzo under the room temperature [a] pyrene is light yellow acicular crystal, can be divided into monoclinic crystal or iris, stable in properties, 310～320 ℃ of boiling points (10mm mercury column), 179～180 ℃ of fusing points, dissolubility is 0.004～0.012mg/L in water, is soluble in cyclohexane extraction, hexane, benzene,toluene,xylene, acetone and other organic solvent, is slightly soluble in ethanol, methanol.Benzo (a) pyrene during with wavelength 360nm ultraviolet radiation, can produce typical purple fluorescence in organic solvent.
Benzo [a] pyrene is found, topmost environment and food contaminant in more than the 200 kind of polycyclic aromatic hydrocarbon.It is the pyrolytic product of carbon-containing fuel and Organic substance, and imperfect combustions such as coal, oil, natural gas, timber all can produce.And these materials have caused the extensive pollution of benzo [a] pyrene in the extensive application of aspects such as industrial and agricultural production, transportation and life.We can say that various of animal or plant nature Chinese crude drugs all may be subjected to the pollution of benzo [a] pyrene.Benzo in most of Chinese crude drugs [a] pyrene is mainly derived from the course of processing of Chinese crude drug.
The fuel that baking is used always in the processing is concocted in the place of production in Chinese medicine village at present coal, Linesless charcoal, coke, coal gas and electric heating etc.Because combustion product directly contacts with Chinese crude drug, the direct contact food of the benzo in the flue dust [a] pyrene and polluting.Because the baking temperature height, compositions such as the fat in the Chinese crude drug, cholesterol can form benzo [a] pyrene through high temperature pyrolysis or hot polymerization.According to research reports, benzo [a] pyrene content is 10～70 times of animal foodstuff itself in the oil droplet that animal foodstuff dripped in the bake process.
Some equipment pipe contains benzo [a] pyrene.As when adopting rubber tubing transferring raw material or finished product, all contain benzo [a] pyrene in the heavy oil of using when the inserts carbon black of rubber and processing rubber, when extracting medicinal liquid through these line transportation, benzo [a] pyrene might be transferred in the extract.
The pollution of industrial wastewater, waste gas: produce carbon black, oil refining, coking, synthetic rubber, the waste water of industries such as burning Colophonium contains a large amount of benzos [a] pyrene in the waste gas, can pollute environment and food.Chinese crude drug is dry in the sun on pitchy highway, and the pitch of fusing can cause benzo [a] pyrene content significantly to increase attached on the grain when temperature was high.When adopting contaminated Chinese crude drug to produce extract, benzo [a] pyrene might be transferred in the extract, causes benzo in the extract [a] pyrene to exceed standard.
Benzo [a] pyrene is a kind of strong carcinogen to the human and animal.Enter human body by water and food, benzo [a] pyrene passes through intestinal absorption very soon.Be distributed in whole body after the absorption very soon.Most internal organs a few minutes and several hours after absorption just can detect benzo [a] pyrene and its metabolite.Can accumulate in mammary gland and the fatty tissue.Benzo [a] pyrene has carcinogenecity and genetoxic, and benzo [a] pyrene of taking at per os can enter the young body of tire by Placenta Hominis, has presented toxicity and carcinogenecity.No matter any approach is taken in, and main excretion pathway is to discharge by feces through liver and gall.The overwhelming majority is its metabolite, has only 1% the prototype that is.Zoopery shows, enters intravital benzo [a] pyrene under the aryl hydrocarbon hydroxylase effect of microsomal mixed function oxidase system, and metabolism activation is the polycyclic aromatic hydrocarbon epoxide, combines with DNA, RNA and protein macromolecule and presents carcinogenesis, becomes ultimate carcinogens.What have can form the chemical compound that has hydroxyl through further metabolism, can combine with glucuronic acid, sulphuric acid or glutathion at last from urine and discharge.
Cause skin carcinoma during initial the discovery, after further investigation, because route of entry and site of action is different, to each internal organs of body such as lung, liver, esophagus, gastrointestinal etc. all can be carcinogenic.There are many epidemiological study data to show the dependency relation of human absorption polynuclear aromatic compound and gastric cancer incidence rate.There is human to contain the forage feed rat 14 months of 20 μ g benzo [a] pyrenes, the most of gastric cancer that takes place of result.The carcinogenic mechanism of benzo [a] pyrene at first is to generate epoxide and phenolic compound under the aryl hydrocarbon hydroxylase effect, further act on epoxides such as generating 7.8-dihydrodiol and 9.10-dihydrodiol at the epoxy hydrase then, deoxidation purine bases in these epoxide and the DNA form adduct, be connected on the nitrogen of guanine or adenine, form N2-deoxy-guanine adduct, N7-deoxy-guanine adduct and N6-deoxyadenine adduct.The carciongenic potency that quantity that these adducts form and persistent period have determined benzo [a] pyrene.
In daily production, can administer, prevent that benzo in the three industrial wastes [a] pyrene from polluting waters, soil, air and plant by environmental enhancement; Change the mode of production, the Chinese crude drug of results is forbidden in the asphalt surface dry in the sun; Improve processing method, avoid composition pyrolysis and hot polymerization as far as possible, prevent that to reduce measures such as benzo [a] pyrene formation benzo [a] pyrene from polluting Chinese medicine extraction.
Benzo [a] pyrene is soluble in cyclohexane extraction, benzene, acetone and other organic solvent, is slightly soluble in ethanol, methanol, so the non-polar solven extraction is effective ways of removing benzo [a] pyrene in the Chinese medicine extract.The Chinese medicine extract major part is with water, the solvent extraction of ethanol isopolarity, and non-polar solven is difficult to infiltrate through in the extract, so the efficient of benzo [a] pyrene is lower in the conventional extraction removal Chinese medicine extract.Superfine communication technique can be crushed to Chinese medicine extract below the diameter 75 μ m, can significantly improve the contact area of extract and non-polar solven, and is significant to improving removal benzo [a] pyrene efficient.
Superfine communication technique is a new technique that grows up in the world over nearly 20 years.So-called micronizing is meant utilizes machinery or hydrokinetic approach that material particles is crushed to process below the particle diameter 100 μ m.Ultramicro powder is the final products of micronizing, has some special physicochemical properties that general granule does not have, as fine solubility, dispersibility, adsorptivity, chemical reactivity etc.Therefore ultramicro powder has been widely used in many fields such as chemical industry, medicine, food, pesticide, cosmetics, dyestuff, coating, electronics, Aero-Space.Superfine communication technique is applied to herbal pharmaceutical gradually recently, and presents good development momentum.The application advantage of micronizing in Chinese medicine is produced is as follows:
" increasing the drug absorption rate, improve its bioavailability " size of drug particle and the structure of powder body is the key factor that influences drug absorption.After Chinese medicine was handled through ultra micro, its granularity is fine and even more, and specific surface area increases, and porosity increases.Medicine can disperse preferably, be dissolved in the gastro-intestinal Fluid, and increases with the contact area of gastrointestinal mucosa, and is easier in gastrointestinal absorption, thereby improved bioavailability greatly.No matter report, be the patch of external if once being arranged, capsule still for oral administration, and all available smaller dose reaches the drug effect of former prescription after micronizing.For the mineral substance medical material, be equivalent to a part and be water-insoluble materials, after ultra micro is handled,, can accelerate its dissolving in vivo because its granularity reduces greatly! Infiltration rate improves its absorbtivity.
" help the retains biological activity composition, improve drug effect " in the micronizing process, can not producing superheating phenomenon through control, even can under low temperature state, carry out, and pulverizing speed is fast, helps keeping the bioactive ingredients and the various nutritional labeling of non-refractory, thereby improves drug effect.As Margarita, add trade union with traditional method and destroy its part composition, and under the purifying gas flow condition of low temperature about-67 ℃ and strictness, carry out micronizing, can fully intactly keep effective ingredient, strengthen its function in delaying senility.Ganoderma contains rich in amino acid and trace element, has effects such as activate immunity function, antitumor, antithrombotic, and after the micronizing, the curative effect performance is more complete.
" conservation is convenient to use " Chinese medicine is after micronizing, and available smaller dose obtains former prescription curative effect.General medicine can no longer pass through processing such as lixiviate, decoction after micronizing, reduced loss of active ingredients in the production link, maximally utilised raw material, so this technology is suitable for the pulverizing of precious rare Chinese medicine especially, and because the increase of fineness, can improve mouthfeel, be convenient to take.On the other hand, in totally-enclosed non-dusting system, carry out, can effectively avoid outside contamination, the content of microorganisms of product and dust are controlled because of micronizing.
Micronizing is a modern advanced, introduces the Chinese medicine manufacture field with the ultra tiny efflorescence of extract, and its grain size of micropowder reaches micron order.Product is the variation of physical property but not chemical change behind the micronization, avoided the change of components in proportions and quantity, increase surface area simultaneously, can significantly improve the contact area of extract and non-polar solven, significant to improving removal benzopyrene efficient.
Summary of the invention
The object of the present invention is to provide a kind of using ultramicro communication technique to remove the method for benzo in the Herba Trifolii Pratentis extract [a] pyrene, this method can significantly improve removes benzo [a] pyrene efficient.
The objective of the invention is to realize in the following manner.
A kind of using ultramicro communication technique removes the method for benzo in the Herba Trifolii Pratentis extract [a] pyrene, with Herba Trifolii Pratentis extract with ethyl acetate and petroleum ether etc. quality extract than stirring solvent hot reflux, to leave standstill the precipitation that obtains after the reflux, extract, through super-dry, pulverize, sieve, mixing promptly gets Herba Trifolii Pratentis extract and takes off benzo [a] pyrene product, before extracting than stirring solvent hot reflux with quality such as ethyl acetate and petroleum ether, Herba Trifolii Pratentis extract is put micronizing in the super micron mill, each 20-30min that pulverizes, particle diameter is no more than 75 μ m, gets the Herba Trifolii Pratentis extract superfine powder and minces.
Dropping into the Herba Trifolii Pratentis extract superfine powder in Alcohol-settling tank minces, stir, extract 4 times 80-90 ℃ of hot reflux, when hot reflux is for the first time extracted used ethyl acetate and petroleum ether etc. quality be 6: 1 than the quality liquid-solid ratio that solvent and Herba Trifolii Pratentis extract superfine powder mince; For the second time when the 4th hot reflux extracted used ethyl acetate and petroleum ether etc. quality be 5: 1 than the quality liquid-solid ratio that solvent and Herba Trifolii Pratentis extract superfine powder mince, the each extraction 1 hour, be cooled to room temperature, make layering to leaving standstill for the third time for the first time, solvent layer, is emitted from bottom after the last stirring cooling from the tank deck siphon, be transferred in the stainless steel cask, leave standstill and made layering in 2 hours; With lower sediment change in the vacuum drying oven reclaim solvent after, vacuum drying gets dry extract; Dry extract is pulverized and mistake 60～80 mesh sieves, mixed, get product.
Detailed process:
1, micronizing: get Herba Trifolii Pratentis extract, put in the super micron mill, carry out, pulverize 20～30min at every turn, detect particle diameter and be no more than 75 μ m by " super micron mill S.O.P. ", standby.
2, extract: in the 2T Alcohol-settling tank, drop into 250～300kg Herba Trifolii Pratentis extract, carry out by " 2T Alcohol-settling tank S.O.P. ", add ethyl acetate and be stirred in 80-90 ℃ of hot reflux with petroleum ether (boiling point is 60～90 ℃) and extract 4 times, during the extraction of hot reflux for the first time used ethyl acetate and petroleum ether etc. quality be 6: 1 than the quality liquid-solid ratio that solvent and Herba Trifolii Pratentis extract superfine powder mince; For the second time when the 4th hot reflux extracted used ethyl acetate and petroleum ether etc. quality be 5: 1 than the quality liquid-solid ratio that solvent and Herba Trifolii Pratentis extract superfine powder mince, the each extraction 1 hour, be cooled to room temperature, make layering to leaving standstill for the third time for the first time, solvent layer, is emitted from bottom after the last stirring cooling from the tank deck siphon, be transferred in the stainless steel cask, leave standstill and made layering in 2 hours; 3, reclaim: the upper strata solvent is drawn in the outer circulation concentrating under reduced pressure device with vacuum carries out by " WZ-1000 outer circulation concentrating under reduced pressure device S.O.P. ", normal pressure reclaims solvent to fully, reclaims residue and places, and is pending.
4, drying: with lower sediment change in the vacuum drying oven reclaim solvent after, vacuum drying gets dry extract.
5, powder, sieve, mixed, bag: 60～80 mesh sieves are pulverized and crossed to dried cream by " the essence baking is wrapped and pulverized, sieves, mixes, packs the post standard operating procedure ", and mixing, packing had both got finished product.
Benzo [a] pyrene is soluble in cyclohexane extraction, benzene, acetone and other organic solvent, is slightly soluble in ethanol, methanol, so the non-polar solven extraction is effective ways of removing benzo [a] pyrene in the Chinese medicine extract.The Chinese medicine extract major part is with water, the solvent extraction of ethanol isopolarity, and non-polar solven is difficult to infiltrate through in the extract, so the efficient of benzo [a] pyrene is lower in the conventional extraction removal Chinese medicine extract.Superfine communication technique can be crushed to Chinese medicine extract below the diameter 75 μ m, can significantly improve the contact area of extract and non-polar solven, and is significant to improving removal benzo [a] pyrene efficient.
Ultramicro powder is the final products of micronizing, has some special physicochemical properties that general granule does not have, as fine solubility, dispersibility, adsorptivity, chemical reactivity etc.After Chinese medicine was handled through ultra micro, its granularity is fine and even more, and specific surface area increases, and porosity increases.Medicine can disperse preferably, be dissolved in the gastro-intestinal Fluid, and increases with the contact area of gastrointestinal mucosa, and is easier in gastrointestinal absorption, thereby improved bioavailability greatly.And in the micronizing process, can not produce superheating phenomenon through control, even can under low temperature state, carry out, and pulverizing speed is fast, helps keeping the bioactive ingredients and the various nutritional labeling of non-refractory, thereby improve drug effect.In addition, in totally-enclosed non-dusting system, carry out, can effectively avoid outside contamination, the content of microorganisms of product and dust are controlled because of micronizing.
Micronizing is a modern advanced, introduces the Chinese medicine manufacture field with the ultra tiny efflorescence of extract, and its grain size of micropowder reaches micron order.Product is the variation of physical property but not chemical change behind the micronization, avoided the change of components in proportions and quantity, increase surface area simultaneously, can significantly improve the contact area of extract and non-polar solven, significant to improving removal benzopyrene efficient.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
Following examples are intended to further specify the present invention, rather than restriction the present invention.
1, micronizing: get Herba Trifolii Pratentis extract, put in the super micron mill, pulverize 30min, detect particle diameter and be no more than 75 μ m, standby.
2, extract: in the 2T Alcohol-settling tank, drop into the 280kg Herba Trifolii Pratentis extract, carry out by " 2T Alcohol-settling tank S.O.P. ", being stirred in 80-90 ℃ of hot reflux extracts 4 times, ethyl acetate and petroleum ether quality such as (60～90 ℃ of boiling points) is 6 times of amounts of Herba Trifolii Pratentis extract micronizing amount for the first time than solvent load, for the second time be 5 times of amounts to the 4th time, the each extraction 1 hour, be cooled to room temperature, make layering to leaving standstill for the third time for the first time, solvent layer is from the tank deck siphon, after the last stirring cooling, emit from bottom, be transferred in the stainless steel cask, leave standstill and made layering in 2 hours.
3, reclaim: the upper strata solvent is drawn in the outer circulation concentrating under reduced pressure device with vacuum carries out by " WZ-1000 outer circulation concentrating under reduced pressure device S.O.P. ", normal pressure reclaims solvent to fully, reclaims residue and places, and is pending.
4, drying: with lower sediment change in the vacuum drying oven reclaim solvent after, vacuum drying gets dry extract.
5, powder, sieve, mixed, bag: 60～80 mesh sieves are pulverized and crossed to dry extract by " the essence baking is wrapped and pulverized, sieves, mixes, packs the post standard operating procedure ", and mixing, packing get product.
Different breaking methods are to the influence of Herba Trifolii Pratentis benzo [a] pyrene clearance
| The experiment number | Benzo [a] pyrene content (ppb) | Breaking method | Take off benzo [a] pyrene thing benzo [a] pyrene content (ppb) | Remove efficient (%) |
| 1 | ?250.6 | Normal method is crushed to 80 orders | 156.0 | 37.6 |
| 2 | ?250.6 | Micronizing 30min | 55.0 | 78.0 |
| 3 | ?246.1 | Normal method is crushed to 80 orders | 165.0 | 32.9 |
| 4 | ?246.1 | Micronizing 30min | 51.2 | 79.2 |
| 5 | ?50.2 | Normal method is crushed to 80 orders | 39.4 | 21.5 |
| 6 | ?50.2 | Micronizing 30min | 12.3 | 75.5 |
Adopt different breaking methods, all the other technological processes are identical with embodiment 1, result of the test shows that benzo [a] the pyrene content of the more common method for making product of content of Herba Trifolii Pratentis extract benzo [a] pyrene in the micronizing afterproduct obviously reduces, and removal efficient is doubled.
Different powder particle diameters are to the influence of Herba Trifolii Pratentis benzo [a] pyrene clearance
| The experiment number | Benzo [a] pyrene content (ppb) | Powder particle diameter | Take off benzo [a] pyrene thing benzo [a] pyrene content (ppb) | Remove efficient (%) |
| 1 | ?150.5 | Be crushed to 150 μ m | 86.2 | 42.7 |
| 2 | ?150.5 | Be crushed to 120 μ m | 65.0 | 56.8 |
| 3 | ?150.5 | Be crushed to 100 μ m | 48.0 | 68.1 |
| 4 | ?150.5 | Be crushed to 75 μ m | 31.6 | 79.0 |
| 5 | ?150.5 | Be crushed to 50 μ m | 30.4 | 79.8 |
Adopt the different pulverizing time, all the other technological processes are identical with embodiment 1, and result of the test shows: the content of Herba Trifolii Pratentis extract benzo [a] pyrene in the micronizing afterproduct reduces along with the minimizing of powder particle diameter; When powder particle diameter when 75 μ m are following, the removal efficient of benzo [a] pyrene no longer increases, so Herba Trifolii Pratentis extract micronizing to particle diameter is no more than 75 μ m, get product by processes such as ethyl acetate and petroleum ether (60～90 ℃ of boiling points) geometric ratio stirring solvent hot reflux extraction, dryings then.
Claims (2)
1. a using ultramicro communication technique removes the method for benzo in the Herba Trifolii Pratentis extract [a] pyrene, with Herba Trifolii Pratentis extract with ethyl acetate and petroleum ether etc. quality extract than stirring solvent hot reflux, to leave standstill the precipitation that obtains after the reflux, extract, through super-dry, pulverize, sieve, mixing promptly gets Herba Trifolii Pratentis extract and takes off benzo [a] pyrene product, it is characterized in that, before extracting than stirring solvent hot reflux with quality such as ethyl acetate and petroleum ether, Herba Trifolii Pratentis extract is put micronizing in the super micron mill, each 20-30min that pulverizes, particle diameter is no more than 75 μ m, gets the Herba Trifolii Pratentis extract superfine powder and minces.
2. using ultramicro communication technique according to claim 1 removes the method for benzo in the Herba Trifolii Pratentis extract [a] pyrene, it is characterized in that, dropping into the Herba Trifolii Pratentis extract superfine powder in Alcohol-settling tank minces, stir, extract 4 times 80-90 ℃ of hot reflux, when hot reflux is for the first time extracted used ethyl acetate and petroleum ether etc. quality be 6: 1 than the quality liquid-solid ratio that solvent and Herba Trifolii Pratentis extract superfine powder mince; For the second time when the 4th hot reflux extracted used ethyl acetate and petroleum ether etc. quality be 5: 1 than the quality liquid-solid ratio that solvent and Herba Trifolii Pratentis extract superfine powder mince, the each extraction 1 hour, be cooled to room temperature, make layering to leaving standstill for the third time for the first time, solvent layer, is emitted from bottom after the last stirring cooling from the tank deck siphon, be transferred in the stainless steel cask, leave standstill and made layering in 2 hours; With lower sediment change in the vacuum drying oven reclaim solvent after, vacuum drying gets dry extract; Dry extract is pulverized and mistake 60～80 mesh sieves, mixed, get product.
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| CN1891242A (en) * | 2005-07-06 | 2007-01-10 | 徐州技源天然保健品有限公司 | Production process for removing polycyclic aromatic hydrocarbons from ginkgo leaf extract |
| CN101273764A (en) * | 2007-03-27 | 2008-10-01 | 高原圣果沙棘制品有限公司 | Method for reducing poisonous substance in seabuckthorn fruit oil and seabuckthorn fruit oil using this method |
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| CN1891242A (en) * | 2005-07-06 | 2007-01-10 | 徐州技源天然保健品有限公司 | Production process for removing polycyclic aromatic hydrocarbons from ginkgo leaf extract |
| CN101273764A (en) * | 2007-03-27 | 2008-10-01 | 高原圣果沙棘制品有限公司 | Method for reducing poisonous substance in seabuckthorn fruit oil and seabuckthorn fruit oil using this method |
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