CN101711777B - Method for removing pesticide residue in production process of lucid ganoderma extract - Google Patents
Method for removing pesticide residue in production process of lucid ganoderma extract Download PDFInfo
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- CN101711777B CN101711777B CN2009103113903A CN200910311390A CN101711777B CN 101711777 B CN101711777 B CN 101711777B CN 2009103113903 A CN2009103113903 A CN 2009103113903A CN 200910311390 A CN200910311390 A CN 200910311390A CN 101711777 B CN101711777 B CN 101711777B
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Abstract
The invention discloses a method for removing a pesticide residue in a production process of a lucid ganoderma extract. The method comprises the following steps of: adding smashed medicinal material of lucid ganoderma into active carbon; extracting the lucid ganoderma by using ethanol; filtering the extracted lucid ganoderma; collecting and extracting a filtrate; condensing the extracted filtrate; adding No.6 solvent oil for extraction and detoxication; and drying, smashing, sieving and mixing to obtain a product of the lucid ganoderma extract with no pesticide residue. The lucid ganoderma extract prepared by the method has a low pesticide residual rate, low cost and simple preparation technology, and is suitable for industrialized mass production.
Description
Technical field
The invention belongs to the Chinese medicine extraction applied technical field, be specifically related to remove in a kind of production process of lucid ganoderma extract the method for pesticide residues.
Background technology
Ganoderma is a basidiomycetes Polyporaceae Ganoderma plant, and its growth course comprises sporophore, mycelium and spore powder three phases.Ganoderma just is considered to a kind of effective strengthening by means of tonics medicine since ancient times, what its application was maximum is the sporophore of Ganoderma, studies show that, the main chemical compositions of Ganoderma has polysaccharide, ucleosides, three-iron acids, sterol, alkaloids and aminoacid etc., and its hypoxia-bearing capability and all many-side such as resisting fatigue and antitumor at calmness, heart tonifying, defying age, raising body has effect widely.Thereby be used to prepare various medicines, food, beverage and cosmetic health product.Ganoderma extract is a raw material with Ganoderma sporophore and Ganoderma spore powder, concentrate drying after solvent extraction and making, and its functional effect is equal to the Ganoderma medical material.
Human civilization enters when developing on an unprecedented scale, and has also brought serious environmental problem.The use of pesticide has caused serious environmental to pollute and direct harm humans health, becomes one of important pollutant that influence environment.Pesticide is made up of organic compound mostly, and its chemical child is stable, and degraded is slowly, and is fat-soluble strong, can be residual at nature for a long time, be easy in biological chain, accumulate roughly serious global environmental pollution, and long-term accumulated can be for decades.The human use by the food of pollution by pesticides, residual pesticide can be accumulated in human body, and the danger that causes people's chronic poisoning is arranged, and the result of long-term hazards to be teratogenesis, carcinogenic, mutagenesis and tardy property, nervous system poison.
Residual pesticide in the at present relevant extract removes technology and generally adopts the high pressure equipment cycling extraction, macroporous resin adsorption, and irradiation under ultraviolet ray etc., as: supercritical CO
2Extraction removes the pesticide residues [publication number: CN1279964A] in the Radix Ginseng extract, the extraction of propane cycle of higher pressure removes [application numbers: CN101156881A] such as pesticide residues in the Radix Ginseng extract, irradiation under ultraviolet ray adds titanium dioxide catalysis, enzyme, Amberlyst process removes pesticide residues in the Radix Ginseng [application number: 94104202.2], and Jilin HongJiu Co., Ltd adopts Amberlyst process to remove pesticide residues [application number: 200710056284.6] etc.Above method is directed to Radix Ginseng extract, and has used big jumbo supercritical or the employing Amberlyst process of production early investment, is not reported and be directed to the patent that removes pesticide residues in the Ganoderma extract.
Summary of the invention
The object of the present invention is to provide the method that removes pesticide residues in a kind of production process of lucid ganoderma extract.
The objective of the invention is to realize in the following manner:
The Ganoderma medical material of the clean no silt of selection, pulverize, cross No. 2 sieves of Chinese Pharmacopoeia, in extraction pot, drop into the Ganoderma medical material that crushes, add active carbon, the ratio that active carbon accounts for Ganoderma medical material grain weight amount is 0.5%～10%, adds 50% alcohol reflux 3 times, filter ethanol extract, extract and abandon after medicinal residues reclaim ethanol, extracting solution reclaims ethanol and gets the Ganoderma extract concentrated solution, changes in the Alcohol-settling tank, adds No. 6 solvent naphthas in concentrated solution, heat of stirring refluxes, standing demix is emitted lower floor's solution and process concentrates, drying, pulverize, sieve, mix, promptly get and hang down agricultural residual Ganoderma extract.
The concentrated solution that described ethanol extract obtains after concentrating and the volume and the weight ratio of Ganoderma medical material powder are 2: 1-1: between 4.
The volume ratio of the concentrated solution that described No. 6 solvent naphthas and ethanol extract obtain after concentrating was not less than 1: 1, and return time is 0.5-3 hour.
Described No. 6 solvent naphthas comprise: the mixed solvent of No. 6 solvents, 120# solvent, petroleum ether, normal hexane, cyclohexane extraction, ethyl acetate and any ratios of wherein any several solvents.
The present invention utilizes similar principle and the adsorption combined technology of mixing, and under fully decentralized solution state, rudimentary property residual pesticide is effectively deviate from.The present invention can improve the efficient that removes the pesticide residues in the Ganoderma extract significantly.On producing, need not large scale investment novel heavy duty equipment, need not equipment is transformed, can make the residual Ganoderma extract of the low farming of reliable quality.The present invention gropes through a large amount of tests, obtains the reaction condition of each step and adds the concentration of solvent, the optimum selection of ratio, can effectively remove the pesticide residues in the Ganoderma extract.It is big to have solved the production early investment, the problem of cost recovery difficulty, solved the security hidden trouble that high pressure equipment brings, solved the problem of ultraviolet radiation to human body harm, solved residual problem of macroporous resin or the like, both replenished original deficiency of taking off agricultural residual technology, and reduced again and taken off the residual cost of farming.
Specific embodiments
Embodiment 1
Get the Ganoderma medical material, pulverize, cross sieve No. 2, in extraction pot, drop into Ganoderma medicated powder 200kg, add 50% ethanol 1600L, stir, heating and refluxing extraction 2 hours, extracting solution is emitted from tank bottoms, adds 50% ethanol 1600L to extraction pot, stir, heating and refluxing extraction 2 hours is emitted extracting solution, adds 50% ethanol 1000L again in extraction pot, stir, heating and refluxing extraction 1 hour is emitted extracting solution, extracts to abandon after slag reclaims ethanol, merge three times extracting solution, change over to and be concentrated into the 50L thick paste in the outer circulation concentrator, again concentrated solution is changed in the vacuum drying oven fully dry, through pulverizing, mix, obtain low agricultural residual Ganoderma extract 23.5kg.Censorship, it is as follows to detect pesticide residues and ganoderan and triterpene:
| Test item | Testing result |
| α-BHC | 14.71ppb |
| β-BHC | 14.44ppb |
| γ-BHC | 12.20ppb |
| PCNB | - |
| δ-BHC | 13.18ppb |
| S421 | 20.84ppb |
| PP’-DDE | 14.18ppb |
| OP’-DDT | 10.18ppb |
| PP’-DDD | 13.24ppb |
| PP’-DDT | 12.18ppb |
| Ganoderan | 12.2％ |
| Triterpene | 4.6％ |
Embodiment 2
Get the Ganoderma medical material, pulverize, cross sieve No. 2, in extraction pot, drop into Ganoderma medicated powder 200kg, add active carbon 10kg, add 50% ethanol 1600L, stir, heating and refluxing extraction 2 hours, extracting solution is emitted from tank bottoms, in extraction pot, add 50% ethanol 1600L, stir heating and refluxing extraction 2 hours, emit extracting solution, in extraction pot, add 50% ethanol 1000L again, stir heating and refluxing extraction 1 hour, emit extracting solution, abandon after extracting slag recovery ethanol, merge three times extracting solution, change over to and be concentrated into the 50L thick paste in the outer circulation concentrator, again concentrated solution is changed in the vacuum drying oven fully dry, through pulverizing, mix, obtain low agricultural residual Ganoderma extract 20.5kg.Censorship, it is as follows to detect pesticide residues and ganoderan and triterpene:
Embodiment 3
Get the Ganoderma medical material, pulverize, cross sieve No. 2, in extraction pot, drop into Ganoderma medicated powder 200kg, add 50% ethanol 1600L, stir, heating and refluxing extraction 2 hours, extracting solution is emitted from tank bottoms, adds 50% ethanol 1600L in extraction pot, stir, heating and refluxing extraction 2 hours is emitted extracting solution, in extraction pot, add 50% ethanol 1000L again, stir heating and refluxing extraction 1 hour, emit extracting solution, abandon after the extraction slag reclaims ethanol, merge three times extracting solution, change over to and be concentrated into the 200L concentrated solution in the outer circulation concentrator, change thick paste over to the Alcohol-settling tank kind, add No. 6 solvent naphtha 2000L, stir, heating and refluxing extraction 2 hours, leave standstill, the thick paste that lower floor's concentrated solution is concentrated into 50L is again analyzed in layering, change in the vacuum drying oven fully dry, through pulverizing, mix, obtain low agricultural residual Ganoderma extract 21.8kg.Censorship, it is as follows to detect pesticide residues and ganoderan and triterpene:
| Test item | Testing result |
| α-BHC | 4.35 |
| β-BHC | 7.26. |
| γ-BHC | 3.19 |
| PCNB | Do not detect |
| δ-BHC | 2.58 |
| S421 | 10.77 |
| PP’-DDE | 1.63 |
| OP’-DDT | 0.84 |
| PP’-DDD | 3.85 |
| PP’-DDT | 5.57 |
| Ganoderan | 12.6％ |
| Triterpene | 4.4％ |
Embodiment 4
Get the Ganoderma medical material, pulverize, cross sieve No. 2, in extraction pot, drop into Ganoderma medicated powder 200kg, add the 10kg active carbon, add 50% ethanol 1600L, stir, heating and refluxing extraction 2 hours, extracting solution is emitted from tank bottoms, in extraction pot, add 50% ethanol 1600L, stir heating and refluxing extraction 2 hours, emit extracting solution, in extraction pot, add 50% ethanol 1000L again, stir heating and refluxing extraction 1 hour, emit extracting solution, abandon after extracting slag recovery ethanol, merge three times extracting solution, change the concentrated solution that is concentrated into 200L in the outer circulation concentrator over to, change in the Alcohol-settling tank, add No. 6 solvent naphtha 2000L, stirring and refluxing was extracted 2 hours, stopped heating and stirring, leave standstill, bottom concentrated solution part is emitted in layering, changes over to and continues to be concentrated into 50L in the concentrator, again concentrated solution is changed in the vacuum drying oven fully dry, through pulverizing, mix, obtain low agricultural residual Ganoderma extract 22.4kg.Censorship, it is as follows to detect pesticide residues and ganoderan and triterpene:
| Test item | Testing result |
| α-BHC | Do not detect |
| β-BHC | Do not detect |
| γ-BHC | Do not detect |
| PCNB | Do not detect |
| δ-BHC | Do not detect |
| S421 | Do not detect |
| PP’-DDE | Do not detect |
| OP’-DDT | Do not detect |
| PP’-DDD | Do not detect |
| PP’-DDT | Do not detect |
| Ganoderan | 12.4％ |
| Triterpene | 4.8％ |
Embodiment 5
Get the Ganoderma medical material, pulverize, cross sieve No. 2, in extraction pot, drop into Ganoderma medicated powder 200kg, add active carbon 1kg, add 50% ethanol 1600L, stir, heating and refluxing extraction 2 hours, extracting solution is emitted from tank bottoms, in extraction pot, add 50% ethanol 1600L, stir heating and refluxing extraction 2 hours, emit extracting solution, in extraction pot, add 50% ethanol 1000L again, stir heating and refluxing extraction 1 hour, emit extracting solution, abandon after extracting slag recovery ethanol, merge three times extracting solution, change over to and be concentrated into the 200L concentrated solution in the outer circulation concentrator, change in the Alcohol-settling tank, add No. 6 solvent naphtha 3000L, stirring and refluxing was extracted 2 hours, stopped heating and stirring, leave standstill, bottom concentrated solution part is emitted in layering, changes over to and continues to be concentrated into 50L in the concentrator, again concentrated solution is changed in the vacuum drying oven fully dry, through pulverizing, mix, obtain low agricultural residual Ganoderma extract 22.8kg.Censorship, it is as follows to detect pesticide residues and ganoderan and triterpene:
Embodiment 6
Get the Ganoderma medical material, pulverize, cross sieve No. 2, in extraction pot, drop into Ganoderma medicated powder 200kg, add active carbon 20kg, add 50% ethanol 1600L, stir, heating and refluxing extraction 2 hours, extracting solution is emitted from tank bottoms, to adding 50% ethanol 1600L, stir heating and refluxing extraction 2 hours, emit extracting solution, in extraction pot, add 50% ethanol 1000L again, stir heating and refluxing extraction 1 hour, emit extracting solution, abandon after extracting slag recovery ethanol, merge three times extracting solution, change over to and be concentrated into the 100L concentrated solution in the outer circulation concentrator, change in the Alcohol-settling tank, add No. 6 solvent naphtha 100L, stirring and refluxing was extracted 3 hours, stopped heating and stirring, leave standstill, bottom concentrated solution part is emitted in layering, changes over to and continues to be concentrated into 50L in the concentrator, again concentrated solution is changed in the vacuum drying oven fully dry, through pulverizing, mix, obtain low agricultural residual Ganoderma extract 19.6kg.Censorship, it is as follows to detect pesticide residues and ganoderan and triterpene:
Claims (3)
1. remove the method for pesticide residues in the production process of lucid ganoderma extract,, filter Ganoderma medical material ethanol extraction after crushed, collect and extract filtrate, concentrate drying, pulverize, sieve, mixing promptly gets Ganoderma extract and takes off the pesticide residues product, it is characterized in that, add active carbon after the Ganoderma pulverizing medicinal materials, use ethanol extraction, filtration concentrates after collecting extracting solution, after adding No. 6 solvent naphtha reflux, extract, in the concentrated solution that obtains again, carry out the once concentration after drying again; The part by weight that described active carbon accounts for Ganoderma medical material powder is 0.5%～10%; The concentrated solution that described ethanol extract obtains after concentrating and the volume and the weight ratio of Ganoderma medical material powder are between 2: 1～1: 4; The volume ratio of the concentrated solution that described No. 6 solvent naphthas and ethanol extract obtain after concentrating was not less than 1: 1.
2. remove the method for pesticide residues in a kind of production process of lucid ganoderma extract according to claim 1, it is characterized in that, described return time is 0.5-3 hour.
3. remove the method for pesticide residues in a kind of production process of lucid ganoderma extract according to claim 1, it is characterized in that described No. 6 solvent naphthas comprise: the mixed solvent of No. 6 solvents, 120# solvent, petroleum ether, normal hexane, cyclohexane extraction, ethyl acetate and any ratios of wherein any several solvents.
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| CN2009103113903A CN101711777B (en) | 2009-12-14 | 2009-12-14 | Method for removing pesticide residue in production process of lucid ganoderma extract |
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| CN2009103113903A CN101711777B (en) | 2009-12-14 | 2009-12-14 | Method for removing pesticide residue in production process of lucid ganoderma extract |
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| CN101711777B true CN101711777B (en) | 2011-06-29 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103202866B (en) * | 2013-03-28 | 2014-06-04 | 宁波立华植物提取技术有限公司 | Method to remove residual pesticide procymidone from ginseng extract |
| CN103156897B (en) * | 2013-03-28 | 2015-05-27 | 宁波立华植物提取技术有限公司 | Method for removing pesticide residue dichloro-diphenyl trichloroethane (DDT) and benzene hexachloride from American ginseng extract |
| CN107335401B (en) * | 2016-12-01 | 2020-07-14 | 上海绿强新材料有限公司 | Method for removing pesticide residues in traditional Chinese medicine ointment formula by using inorganic adsorbent |
| CN109289307B (en) * | 2018-10-26 | 2020-12-22 | 劲牌生物医药有限公司 | Method for removing plasticizer from extract |
| CN109464473A (en) * | 2018-11-29 | 2019-03-15 | 杨凌萃健生物工程技术有限公司 | A kind of residual ganodenic acid extract of low agriculture and preparation method thereof |
| CN109481478A (en) * | 2018-11-29 | 2019-03-19 | 杨凌萃健生物工程技术有限公司 | A kind of residual ganoderan extract of low agriculture and preparation method thereof |
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