CN107335401A - A kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent - Google Patents

A kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent Download PDF

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CN107335401A
CN107335401A CN201611088410.1A CN201611088410A CN107335401A CN 107335401 A CN107335401 A CN 107335401A CN 201611088410 A CN201611088410 A CN 201611088410A CN 107335401 A CN107335401 A CN 107335401A
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inorganic adsorbent
paste
herbal paste
traditional chinese
medical science
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CN107335401B (en
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余金鹏
王鹏飞
徐华胜
朱琳
陈保华
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SHANGHAI LUQIANG NEW MATERIALS CO Ltd
Shanghai Research Institute of Chemical Industry SRICI
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SHANGHAI LUQIANG NEW MATERIALS CO Ltd
Shanghai Research Institute of Chemical Industry SRICI
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/165—Natural alumino-silicates, e.g. zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials

Abstract

The present invention relates to a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent, comprise the following steps：(1) inorganic adsorbent is prepared in the inorganic material such as the molecular sieves of ZSM 5, magnalium hydrotalcite；(2) rare medicinal herbs in herbal paste and common medicinal material are separately extracted, after crushing respectively, adds water, add inorganic adsorbent, extraction is stirred in heating, and filtering stays extract solution, the dregs of a decoction are extracted again；(3) rare medicinal herbs extract solution and common herbal extract are merged, are placed in low pressure enrichment facility, heated, concentration, add paste making agent, herbal paste is made.The inventive method is easy, more suitable for the herbal paste Making programme of " side of a people one "；Inorganic adsorbent used in the present invention, safe to use, the residues of pesticides in energy selectively removing herbal paste extract solution, and herbal paste active ingredient is not adsorbed；Compared with traditional herbal paste preparation method, extraction time is shortened, reduces thickening temperature, it is more preferable to retain thermal sensitivity active ingredient.

Description

A kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent
Technical field
The invention belongs to Chinese medicine, Chinese patent drug to remove exogenous nuisance field, and inorganic adsorbent is utilized more particularly, to one kind The method that agent removes traditional Chinese medical science herbal paste Pesticide Residues.
Background technology
Traditional Chinese medical science herbal paste, also referred to as paste, cream are grown, and are the traditional Chinese medicine formulations that Ancient Times in China is handed down, and are eaten in a manner of for oral administration With.Traditional Chinese medical science herbal paste can not only nourish constitution, even more treat the effective means of chronic disease.With China's rapid economic development, city City's sub-health population is increasing, while aging population is serious all the more, and chronic diseases in China people is on the increase, and has made a definite diagnosis at present Rejuvenation trend is presented more than 300,000,000 in chronic patient.Therefore, herbal paste is increasingly favored by people, and the winter takes herbal paste and entered The number of benefit rises year by year.Traditional Chinese medical science herbal paste is very universal in China river, Zhejiang, the band of Shanghai one, and progressively to the other regional developments in China. In addition in China Hong Kong, Macao, Taiwan and the band of Southeast Asia one, herbal paste use is even more like a raging fire, in the ascendant.
However, part medicinal herbs most in use in herbal paste, mostly artificial growth, such as ginseng, the Radix Astragali, matrimony vine, radix glycyrrhizae, often containing more Kind pesticide residue.(discussion [J] CHINA JOURNAL OF CHINESE MATERIA MEDICAs .2016,41 (02) of the residual present Research of the Chinese medicine agricultures such as Kang Chuanzhi: 155-159).In herbal paste manufacturing process, pesticide residue contained by medicinal material can enter in herbal paste, so as to pollute herbal paste.The opposing party Face, herbal paste need long-term use of (general 2~3 months)；If the long-term use of this herbal paste by pesticide residue pollution, to user The potential hazard that body presence can not be estimated.
At present, it is domestic to there is no the document report removed to traditional Chinese medical science herbal paste Pesticide Residues thing and related publication. Only several patents are related to the removing of single medicinal material material or Chinese medical extract residues of pesticides, can be divided into following four according to removing principle Class：(1) supercritical CO2Extraction：Chinese patent CN1319545C, CN103305343B utilize supercritical CO2Extraction removes respectively Organo-chlorine pesticide, organophosphorus pesticide in ginseng, tangerine oil.(2) subcritical fluid extraction method：Chinese patent CN103549236A removes the residues of pesticides of plant surface attachment using DC naphtha propane etc..(3) macroreticular resin absorbing method：In State's patent CN103739731A, CN104490966A is stripped of lentinan extract, people each with macroporous resin adsorption post Join the residues of pesticides in stem-leaf extract.(4) active carbon adsorption：Chinese patent CN101731493A, CN101711777B profit Ginkgo biloba p.e, Ganodenna Lucidum P.E Pesticide Residues are reduced with charcoal absorption.
Traditional Chinese medical science herbal paste prescription is varied from because body is different, is customized more by hospital pharmacy, every batch of medicinal material amount does not surpass Cross 5 kilograms.Supercritical CO2Extraction, subcritical fluid extraction method need to use high-tension apparatus, be not easy to promote the use of.Herbal paste is more Being boiled with water, macroreticular resin, activated carbon etc. are nonpolar, if being directly used in adsorbing and removing herbal paste extract solution Pesticide Residues, The loss of active ingredient can be caused.Therefore, its Pesticide Residues can effectively be removed during herbal paste boils by being badly in need of exploitation one kind Selective absorbent, while residues of pesticides are removed, active ingredient in herbal paste is not adsorbed, so that herbal paste Pesticide Residues Thing is reduced within safety limit.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind utilizes inorganic adsorbent The method that agent removes traditional Chinese medical science herbal paste Pesticide Residues, the inventive method retain herbal paste while herbal paste Pesticide Residues are removed Active ingredient.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent, is comprised the following steps：
(1) preparation of inorganic adsorbent；
(2) rare medicinal herbs in herbal paste and common medicinal material are separately extracted, respectively with after crushing crusher machine, adds water, add Step (1) described inorganic adsorbent, is placed in heating water bath equipment, heating, and extract solution is stayed in stirring extraction, filtering, by the dregs of a decoction again Secondary extraction；
(3) the rare medicinal herbs extract solution of step (2) is merged with common herbal extract, is placed in low pressure concentration dress In putting, heat, concentration, add paste making agent, herbal paste is made.
The preparation of inorganic adsorbent specifically uses following steps in the step (1)：
After (1-1) activates ZSM-5 molecular sieve original powder, ZSM-5 molecular sieve activation powder is cooled down to obtain；
After (1-2) activates magnalium hydrotalcite original powder, magnalium hydrotalcite activation powder is cooled down to obtain；
ZSM-5 molecular sieve is activated powder by (1-3), magnalium hydrotalcite activation powder mixes, and adds a small amount of water, activated alumina is made For binding agent, after being sufficiently mixed, with extruder extruded moulding, reactivation, it is stored in standby in dry environment.
The silica alumina ratio 5~50 of ZSM-5 molecular sieve, preferably silica alumina ratio 10~25 in the step (1-1).
ZSM-5 molecular sieve activation powder in the step (1-3), magnalium hydrotalcite activation both powder mass ratio for (0.1~ 1):(0.1~1), activated alumina quality be ZSM-5 molecular sieve activate powder and magnalium hydrotalcite activate silty amount and 1/5.
ZSM-5 molecular sieve original powder activation condition is 250~450 DEG C in step (1-1), activates more than 1 hour, preferably activates Condition is：Activated 2~4 hours at 350~400 DEG C of temperature；
Magnalium hydrotalcite original powder activation condition is 250~400 DEG C in step (1-2), activates more than 1 hour, preferably activates Condition is：Activated 2~4 hours at 350~400 DEG C of temperature；
Step (1-3) extruded moulding post activation condition is 250~400 DEG C and activated more than 1 hour that preferably activation condition is： Activated 2~4 hours at 350~400 DEG C of temperature.
The rare medicinal herbs includes the one or more in ginseng, red ginseng, pseudo-ginseng, ganoderma lucidum；The rare medicinal herbs is crushed to Pass through 10 mesh standard sieve nets；During the rare medicinal herbs extraction, it is 15 liter/kilogram medicinal materials to add water first, second of addition water Measure as 14 liter/kilogram medicinal materials, add inorganic adsorbent dosage and run after fame the 1/100~1/50 of precious medicinal material quality, water bath heating temperature 60 ~90 DEG C, preferably 70 DEG C, each more than 1 hour heating water bath time, preferably 2~3 hours.
The common medicinal material is other medicinal materials in addition to rare medicinal herbs, and the common medicinal material is crushed to accurate by 10 targets Screen cloth；During the common medicinal material extract, it is 10 liter/kilogram medicinal materials to add water first, and it is 9 liters/kilogram that second, which adds water, Medicinal material, addition inorganic adsorbent dosage are the 1/50~1/20 of common quality of medicinal material, 60~100 DEG C of water bath heating temperature, preferably 80 DEG C, each more than 0.5 hour heating water bath time, preferably 1~2 hour.
The residues of pesticides species of the herbal extract Pesticide Residues thing, wherein inorganic adsorbent energy adsorbing and removing and dense Degree scope includes：0.005~1.0mg/L of pentachloronitrobenzene, total 0.001~0.5mg/L of BHC, total DDT 0.001~ 0.5mg/L, 0.005~1.0mg/L of flolimat, 0.005~1.0mg/L of parathion-methyl, 0.005~1.0mg/ of cypermethrin L, the one or more in 0.005~1.0mg/L of fenvalerate, 0.005~1.0mg/L of cyfloxylate.
The low pressure enrichment facility is the Rotary Evaporators with heater block and vacuum pump part, heating-up temperature 40~80 DEG C, rotavapor under vacuum degree is 60~95kPa；The volume of concentrate is the 1/10~1/5 of extracting liquid volume.
The paste making agent is the one or more in white sugar, xylitol, rock sugar, honey, and paste making agent dosage is every liter of concentration 0.1~0.3 kilogram of liquid addition paste.
It is of the invention to make work with existing single medicinal material material or the removing sulfuldioxide of Chinese medical extract residues of pesticides and traditional herbal paste Skill is compared, and has advantages below：
(1) the method for the invention is easy, more suitable for the herbal paste Making programme of " side of a people one ".Traditional Chinese medical science herbal paste prescription because Body is different and is varied from, and every batch of medicinal material amount is less, and processing batch is more.Supercritical CO2Extraction, subcritical fluids extraction High-tension apparatus need to be used by following the example of, and be not easy to promote.The method of the invention need to only add in herbal paste decoction process with medicinal material Enter inorganic adsorbent, you can reach adsorbing and removing residues of pesticides effect, without increasing any extras.
(2) adsorbent main component of the present invention is artificial synthesized inorganic porous material, safe to use, can selectivity The residues of pesticides in herbal paste extract solution are removed, and do not adsorb herbal paste active ingredient substantially.Macroreticular resin is high molecular polymer, one As can only be used under less than 40 DEG C environment.When temperature in use is higher than 70 DEG C, macroreticular resin can degrade and discharge poisonous Material.In addition, macroreticular resin and activated carbon all have macroporous structure (>50nm), and to be nonpolar, easily adsorb in herbal paste effectively into Point, so as to influence herbal paste curative effect.Inorganic adsorbent main component of the present invention is ZSM-5 molecular sieve and magnalium hydrotalcite. ZSM-5 molecular sieve is alumino-silicate composition, molecular formula Nan(H2O)16[AlnSi96-nO192] (wherein n<27).Magnalium hydrotalcite For layered bi-metal oxide, molecular formula Mg6Al2(OH)16CO3·4H2O.Both materials can be in room temperature~100 DEG C environment Middle safe handling, noxious material will not be discharged.In addition, the polarity of ZSM-5 molecular sieve can be adjusted by silica alumina ratio, silica alumina ratio 10~ ZSM-5 is close with pesticide molecule polarity when 25, can selective absorption herbal paste extract solution Pesticides molecule.The interlayer of magnalium hydrotalcite Away from for 0.4~0.8nm, and pesticide molecule adjoining dimensions, and in herbal paste the general molecular dimension of active ingredient it is larger (>2nm).Cause This, magnalium hydrotalcite can pass through size sieving actoion adsorbing and removing herbal paste Pesticides molecule.
(3) herbal paste preparation method of the present invention shortens extraction time compared with traditional herbal paste preparation method, reduces dense Contracting temperature, it is more preferable to retain thermal sensitivity active ingredient.In traditional herbal paste manufacturing process, medicinal material need to often soak more than 8 hours, then start Decoct.The present invention will directly decoct after pulverizing medicinal materials, save soak time, and powdered medicinal material only needs shorter decocting time. Traditional herbal paste concentration process, simmered for a long time using slow fire, the present invention utilizes low pressure concentration technique, heating-up temperature relatively low 40~80 DEG C, be advantageous to retain thermal sensitivity active ingredient, and the time required to concentration process also further shorten.
Embodiment
Using the method for inorganic adsorbent removing traditional Chinese medical science herbal paste Pesticide Residues, comprise the following steps：
(1) preparation of inorganic adsorbent；
(2) rare medicinal herbs in herbal paste and common medicinal material are separately extracted, respectively with after crushing crusher machine, adds water, add Step (1) described inorganic adsorbent, is placed in heating water bath equipment, heating, and extract solution is stayed in stirring extraction, filtering, by the dregs of a decoction again Secondary extraction；
(3) the rare medicinal herbs extract solution of step (2) is merged with common herbal extract, is placed in low pressure concentration dress In putting, heat, concentration, add paste making agent, herbal paste is made.
The preparation of inorganic adsorbent specifically uses following steps in step (1)：
(1-1) through 250~450 DEG C, activates ZSM-5 molecular sieve original powder more than 1 hour, cools down to obtain ZSM-5 molecular sieve work Change powder；The silica alumina ratio 5~50 of 350~400 DEG C of preferable temperature, preferably 2~4 hours time, wherein ZSM-5 molecular sieve, preferably silicon Aluminum ratio 10~25；
(1-2) through 250~400 DEG C, activates magnalium hydrotalcite original powder more than 1 hour, cools down to obtain magnalium hydrotalcite activation Powder；350~400 DEG C of preferable temperature, preferably 2~4 hours time；
ZSM-5 molecular sieve is activated powder by (1-3), magnalium hydrotalcite activation powder mixes, and adds a small amount of water, activated alumina is made For binding agent, both ZSM-5 molecular sieve activation powder, magnalium hydrotalcite activation powder mass ratio are (0.1~1):(0.1~1), activity Quality of alumina be ZSM-5 molecular sieve activate powder and magnalium hydrotalcite activate silty amount and 1/5, after being sufficiently mixed, with extrusion Machine extruded moulding, activate more than 1 hour, be stored in standby in dry environment in 250~400 DEG C；It is preferred that activation temperature 350~ 400 DEG C, preferably soak time 2~4 hours.
Wherein rare medicinal herbs includes the one or more in ginseng, red ginseng, pseudo-ginseng, ganoderma lucidum；The rare medicinal herbs is crushed to Pass through 10 mesh standard sieve nets；During the rare medicinal herbs extraction, it is 15 liter/kilogram medicinal materials to add water first, second of addition water Measure as 14 liter/kilogram medicinal materials, add inorganic adsorbent dosage and run after fame the 1/100~1/50 of precious medicinal material quality, water bath heating temperature 60 ~90 DEG C, preferably 70 DEG C, each more than 1 hour heating water bath time, preferably 2~3 hours.
Common medicinal material is other medicinal materials in addition to rare medicinal herbs, and the common medicinal material is crushed to by 10 mesh standard sieves Net；During the common medicinal material extract, it is 10 liter/kilogram medicinal materials to add water first, and it is 9 liter/kilogram medicines that second, which adds water, Material, addition inorganic adsorbent dosage are the 1/50~1/20 of common quality of medicinal material, 60~100 DEG C of water bath heating temperature, preferably 80 DEG C, Each more than 0.5 hour heating water bath time, preferably 1~2 hour.
Low pressure enrichment facility is the Rotary Evaporators with heater block and vacuum pump part, 40~80 DEG C of heating-up temperature, Rotavapor under vacuum degree is 60~95kPa；The volume of concentrate is the 1/10~1/5 of extracting liquid volume.
Paste making agent is the one or more in white sugar, xylitol, rock sugar, honey, and paste making agent dosage is that every liter of concentrate adds 0.1~0.3 kilogram of paste making agent.
The residues of pesticides species and concentration range of inorganic adsorbent energy adsorbing and removing include pentachloronitrobenzene (0.005~ 1.0mg/L), total BHC (0.001~0.5mg/L), total DDT (0.001~0.5mg/L), flolimat (0.005~ 1.0mg/L), parathion-methyl (0.005~1.0mg/L), cypermethrin (0.005~1.0mg/L), fenvalerate (0.005~ 1.0mg/L), the one or more in cyfloxylate (0.005~1.0mg/L).
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1 joins the preparation of art cream
The preparation of inorganic adsorbent：0.1 kilogram of ZSM-5 molecular sieve original powder (ZSM-5 silica alumina ratios are 10.3) is placed in 250 Activated 4 hours in DEG C Muffle furnace, taking-up, which is put in drier, to be cooled down；1 kilogram of magnalium hydrotalcite original powder is placed in 400 DEG C of Muffle furnaces Middle activation 2 hours, taking-up, which is put in drier, to be cooled down；By above two material, and 0.22 kilogram of activated alumina is added, stirring Mix, while adding a small amount of water makes powder surface have moist feeling, using extruder, is extruded into 1.8 millimeters of fine strip shape, is placed in Activated 4 hours in 250 DEG C of Muffle furnace, taking-up, which is put in drier, to be cooled down, standby.
Join the extraction of art cream：The prescription for joining art cream is 120 grams of ginseng (going reed), 240 grams of the bighead atractylodes rhizome (soil is fried), stir-fry coix seed 120 grams, 90 grams of lotus-seed kernel (peeling, coring), 90 grams of the Radix Astragali (honey is processed), 60 grams of PORIA ALBA (peeling), 60 grams of Divine Comedy (stir-fry), rhizoma alismatis 9 Gram, 9 grams of honey-fried licorice root.Wherein ginseng is rare medicinal herbs, need to individually be extracted, and remaining medicinal material is common medicinal material, can be extracted together.Will 120 grams of ginsengs are crushed to by 10 mesh standard sieves with food crusher, add 1.8 liters of water, add 1.2 grams of inorganic adsorbents, water 60 DEG C of bath heating, stirring extraction 3 hours；Filter to get filtrate about 1.6 liters；Filter residue adds 1.68 liters of water and extracted again, heating water bath To 60 DEG C, stirring extraction 3 hours, filter to get filtrate about 1.5 liters；Merge to obtain 3.1 liters of extract solutions.Remaining eight kinds common medicinal materials are total to 678 grams, 10 mesh sieves are each crushed, are mixed, add 6.8 liters of water, 13.6 grams of inorganic adsorbents is added, 60 DEG C of heating water bath, stirs Mix extraction 2 hours；Filter to get filtrate 5.3 liters；Filter residue adds 6.1 liters of water and extracted again, and heating water bath is to 60 DEG C, stirring extraction 2 Hour, filter to get filtrate about 5.1 liters；Merge to obtain 10.4 liters of extract solutions.Ginseng extract is mixed with other herbal extracts 13.5 rise extract solution.
Join the concentration of art cream with into cream：13.5 liters of extract solutions are added in Rotary Evaporators in batches, 40 DEG C of heating-up temperature, Vacuum 95kPa；1.35 liters are concentrated into, adds 0.135 kilogram of white sugar while hot, thick ginseng art is formed after being sufficiently stirred dissolving Cream.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, chlorine cyanogen chrysanthemum in tandem mass spectrometry measure ginseng art cream 8 kinds of persticide residues such as ester, fenvalerate, cyfloxylate, do not detect, are shown in Table 1.Compared with comparative example 1, nothing used in explanation Machine adsorbent has preferable removal effect to this 8 kinds of residues of pesticides.Compared with comparative example 2, inorganic adsorbent is to agriculture used in explanation Medicine residue removal effect is better than activated carbon.
According to《Chinese Pharmacopoeia 2015 editions》In the first volume《Ginseng》, join total people in art cream using high effective liquid chromatography for measuring Ginseng saponin content is 521mg/L.Compared with comparative example 1, inorganic adsorbent used in explanation does not cause the loss of general ginsenoside.With Comparative example 2 is compared, and inorganic adsorbent used in explanation does not adsorb effective ingredient, and activated carbon can cause effective ingredient It is lost in.
The conventional method of comparative example 1 prepares ginseng art cream
Join the extraction of art cream：Join the prescription of art cream with embodiment 1.Wherein ginseng individually extracts, and remaining medicinal material merges together Extraction.120 grams of ginsengs are cut into slices, add 5 liters of water, soaks 8 hours, is cooked by slow fire after being boiled by fire 4 hours；Filter to get filtrate about 3 liters of extract solutions.By totally 678 grams of remaining eight kinds of medicinal material, trimming or segment, mixing, 15 liters of water are added, soak 8 hours, be boiled by fire After be cooked by slow fire 4 hours；Filter to get filtrate about 10 liters of extract solutions.Ginseng extract is mixed to obtain 13 liters with other herbal extracts Extract solution.
Join the concentration of art cream with into cream：13 liters of extract solution slow fire are concentrated into 1.35 liters, add white sugar 0.135 thousand while hot Gram, form thick ginseng art cream after being sufficiently stirred dissolving.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, chlorine cyanogen chrysanthemum in tandem mass spectrometry measure ginseng art cream 8 kinds of persticide residues such as ester, fenvalerate, cyfloxylate.Compared with Example 1,8 kinds of residues of pesticides have inspection in herbal paste Go out, specific data are shown in Table 1.
According to《Chinese Pharmacopoeia 2015 editions》In the first volume《Ginseng》, join total people in art cream using high effective liquid chromatography for measuring Ginseng saponin content is 440mg/L.Compared with Example 1, total Ginsenosides Content has declined, it may be possible to due in sheet ginseng Ginsenoside extraction is not exclusively and the heat time is longer caused.
Activated carbon is prepared ginseng art cream by comparative example 2
Join the extraction of art cream, concentration, into cream process with embodiment 1.Inorganic adsorbent used is only changed to etc. to the doctor of quality Use Powdered Activated Carbon.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, chlorine cyanogen chrysanthemum in tandem mass spectrometry measure ginseng art cream 8 kinds of persticide residues such as ester, fenvalerate, cyfloxylate.Compared with embodiment 1, comparative example 1, illustrate activated carbon to 8 kinds Residues of pesticides also have certain adsorbing and removing effect, but adsorbing and removing effect is not as good as inorganic adsorbent used in embodiment 1, specifically Data are shown in Table 1.
According to《Chinese Pharmacopoeia 2015 editions》In the first volume《Ginseng》, join total people in art cream using high effective liquid chromatography for measuring Ginseng saponin content is 461mg/L.Compared with Example 1, total Ginsenosides Content has declined, and illustrates that activated carbon can cause Chinese medicine The loss of active ingredient.
The testing result of table 1
Embodiment 2 joins the preparation of Siberian cocklebur lagehead atractylodes paste
The preparation of inorganic adsorbent：1 kilogram of ZSM-5 molecular sieve original powder (ZSM-5 silica alumina ratios are 24.6) is placed in 450 DEG C Activated 2 hours in Muffle furnace, taking-up, which is put in drier, to be cooled down；0.1 kilogram of magnalium hydrotalcite original powder is placed in 250 DEG C of Muffle furnaces Middle activation 4 hours, taking-up, which is put in drier, to be cooled down；By above two material, and 0.22 kilogram of activated alumina is added, stirring Mix, while adding a small amount of water makes powder surface have moist feeling, using extruder, is extruded into 1.8 millimeters of fine strip shape, is placed in Activated 2 hours in 400 DEG C of Muffle furnace, taking-up, which is put in drier, to be cooled down, standby.
Join the extraction of Siberian cocklebur lagehead atractylodes paste：It is 200 grams of ginseng, 200 grams of PORIA ALBA, 200 grams of radix glycyrrhizae, the bighead atractylodes rhizome to join Siberian cocklebur lagehead atractylodes paste prescription 200 grams, 200 grams of Chinese yam, 150 grams of Semen Lablab Album (ginger juice soak, micro- stir-fry), 100 grams of Semen Nelumbinis, 100 grams of coix seed, 100 grams of contracting fructus amomi, 100 grams of balloonflower root.By ginseng, 200 grams are crushed to by 10 mesh sieves, add 3 liters of water, add 4 grams of inorganic adsorbents, heating water bath 90 DEG C, stirring extraction 2 hours；Filter to get filtrate 2.6 liters；Filter residue adds 2.8 liters of water and extracted again, and heating water bath is to 90 DEG C, stirring Extraction 2 hours, filters to get filtrate about 2.5 liters；Merge to obtain 5.1 liters of extract solutions.Remaining nine kinds of medicinal material crushed 10 for totally 1350 grams Mesh sieve, 13.5 liters of water are added, add 67.5 grams of inorganic adsorbents, 100 DEG C of heating water bath, stirring extraction 1 hour；Filter to get filtrate 10.5 liters；Filter residue adds 12.2 liters of water and extracted again, 100 DEG C of heating water bath, stirring extraction 1 hour, filters to get filtrate 10 liters；Close And obtain 20.5 liters of extract solutions.Two kinds of extract solutions are mixed into obtain 25.6 liters of extract solutions.
Join the concentration of Siberian cocklebur lagehead atractylodes paste with into cream：25.6 liters of extract solutions are added in Rotary Evaporators in batches, heating-up temperature 80 DEG C, vacuum 60kPa；5.1 liters are concentrated into, adds 1.53 kilograms of rock sugar while hot, thick ginseng is formed after being sufficiently stirred dissolving Siberian cocklebur lagehead atractylodes paste.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, chlorine in tandem mass spectrometry measure ginseng Siberian cocklebur lagehead atractylodes paste 8 kinds of persticide residues such as Cyano chrysanthemate, fenvalerate, cyfloxylate, do not detect, are shown in Table 2.
According to《Chinese Pharmacopoeia 2015 editions》In the first volume《Ginseng》, joined using high effective liquid chromatography for measuring in Siberian cocklebur lagehead atractylodes paste Total content of ginsenoside is 268mg/L.Compared with comparative example 3, inorganic adsorbent used in explanation does not adsorb effective ingredient, and D101 macroreticular resins can cause the loss of effective ingredient.
Comparative example 3 prepares ginseng Siberian cocklebur lagehead atractylodes paste by the use of D101 macroreticular resins as adsorbent
Join the extraction of Siberian cocklebur lagehead atractylodes paste, concentration, into cream process with embodiment 2.Inorganic adsorbent used such as is only changed at the quality D101 macroreticular resins (in terms of macroreticular resin dry weight).
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, chlorine in tandem mass spectrometry measure ginseng Siberian cocklebur lagehead atractylodes paste 8 kinds of persticide residues such as Cyano chrysanthemate, fenvalerate, cyfloxylate, detect wherein three kinds of residues of pesticides.With the phase of embodiment 2 Than illustrating that D101 macroreticular resins are shown in Table 2 to residues of pesticides removal effect not as good as the inorganic adsorbent, specific data.
According to《Chinese Pharmacopoeia 2015 editions》In the first volume《Ginseng》, joined using high effective liquid chromatography for measuring in Siberian cocklebur lagehead atractylodes paste Total content of ginsenoside is 212mg/L.Compared with Example 2, illustrate that D101 macroreticular resins can cause the stream of effective ingredient Lose.
The testing result of table 2
The preparation of the lagehead atractylodes paste of embodiment 3
The preparation of inorganic adsorbent：0.5 kilogram of ZSM-5 molecular sieve original powder (silica alumina ratio 19.6) is placed in 350 DEG C of Muffles Activated 1 hour in stove, taking-up, which is put in drier, to be cooled down；0.5 kilogram of magnalium hydrotalcite original powder is placed in 350 DEG C of Muffle furnaces living Change 1 hour, taking-up, which is put in drier, to be cooled down；By above two material, and 0.2 kilogram of activated alumina is added, stirred and evenly mixed, Add a small amount of water simultaneously and powder surface is had moist feeling, using extruder, be extruded into 1.8 millimeters of fine strip shape, be placed in 350 DEG C Activated 1 hour in Muffle furnace, taking-up, which is put in drier, to be cooled down, standby.
The extraction of lagehead atractylodes paste：The prescription of lagehead atractylodes paste is 500 grams of the bighead atractylodes rhizome, 120 grams of dried orange peel.Both are common drug material.Will be white Art, dried orange peel crushed 10 mesh sieves respectively.Two kinds of herb in granule form mixing, add 6.2 liters of water, add 25 grams of inorganic adsorbents, water-bath 80 DEG C of heating, stirring extraction 0.5 hour；Filter to get filtrate 5 liters；Filter residue adds 5.6 liters of water and extracted again, heating water bath to 80 DEG C, stirring extraction 0.5 hour, filter to get filtrate about 4.8 liters；Merge to obtain 9.8 liters of extract solutions.
The concentration of lagehead atractylodes paste with into cream：9.8 liters of extract solutions are added in Rotary Evaporators in batches, 60 DEG C of heating-up temperature, Vacuum 80kPa；1.9 liters are concentrated into, adds 0.57 kilogram of xylitol while hot, the thick bighead atractylodes rhizome is formed after being sufficiently stirred dissolving Cream.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Tandem mass spectrometry measure wherein pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, cypermethrin, 8 kinds of persticide residues such as fenvalerate, cyfloxylate, are not detected.
The preparation of the medlar oil of embodiment 4
The preparation of inorganic adsorbent：0.5 kilogram of ZSM-5 molecular sieve original powder (silica alumina ratio 15.2) is placed in 400 DEG C of Muffles Activated 1 hour in stove, taking-up, which is put in drier, to be cooled down；0.5 kilogram of magnalium hydrotalcite original powder is placed in 400 DEG C of Muffle furnaces living Change 1 hour, taking-up, which is put in drier, to be cooled down；By above two material, and 0.2 kilogram of activated alumina is added, stirred and evenly mixed, Add a small amount of water simultaneously and powder surface is had moist feeling, using extruder, be extruded into 1.8 millimeters of fine strip shape, be placed in 400 DEG C Activated 1 hour in Muffle furnace, taking-up, which is put in drier, to be cooled down, standby.
The extraction of medlar oil：The prescription of medlar oil is 1000 grams of matrimony vine, 60 grams of the fruit of Chinese magnoliavine.Matrimony vine and the fruit of Chinese magnoliavine are common Medicinal material.Matrimony vine, the fruit of Chinese magnoliavine be crushed into 10 mesh sieves respectively.After both mixing, 10.6 liters of water are added, add 30 grams of inorganic adsorbents Agent, 80 DEG C of heating water bath, stirring extraction 1.5 hours；Filter to get filtrate 8.5 liters；Filter residue adds 9.5 liters of water and extracted again, water-bath 80 DEG C are heated to, stirring extraction 1.5 hours, is filtered to get filtrate about 8.5 liters；Merge to obtain 17 liters of extract solutions.
The concentration of medlar oil with into cream：17 liters of extract solutions are added in Rotary Evaporators in batches, 60 DEG C of heating-up temperature, very Reciprocal of duty cycle 80kPa；2 liters are concentrated into, adds 0.4 kilogram of rock sugar while hot, thick medlar oil is formed after being sufficiently stirred dissolving.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Tandem mass spectrometry measure wherein pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, cypermethrin, 8 kinds of persticide residues such as fenvalerate, cyfloxylate, are not detected.
The preparation of 5 liang of instrument cream of embodiment
The preparation of inorganic adsorbent：It is small that 0.5 kilogram of ZSM-5 molecular sieve original powder is placed in activation 1 in 400 DEG C of Muffle furnaces When, taking-up, which is put in drier, to be cooled down；0.5 kilogram of magnalium hydrotalcite original powder is placed in 400 DEG C of Muffle furnaces and activated 1 hour, is taken Go out to be put in drier and cool down；By above two material, and 0.2 kilogram of activated alumina is added, stirred and evenly mixed, while added few Amount water makes powder surface have moist feeling, using extruder, is extruded into 1.8 millimeters of fine strip shape, is placed in 400 DEG C of Muffle furnace living Change 1 hour, taking-up, which is put in drier, to be cooled down, standby.
The extraction of two instrument cream：The prescription of two instrument cream is 250 grams of ginseng, 250 grams of big cultivated land.By ginseng, 250 grams crushed 10 Mesh sieve, 3.75 liters of water are added, add 5 grams of inorganic adsorbents, 70 DEG C of heating water bath, extract 1 hour；Filter to get filtrate 3.1 liters；Filter Slag adds 3.5 liters of water and extracted again, and heating water bath stirring extraction 1 hour, filters to get filtrate about 3.1 liters to 70 DEG C；Merge 6.2 liters of extract solutions.Big 250 grams of cultivated land be crushed into 10 mesh sieves, add 2.5 liters of water, add 5 grams of inorganic adsorbents, heating water bath 80 DEG C, stirring extraction 1 hour；Filter to get filtrate 2 liters；Filter residue adds 2.25 liters of water and extracted again, and 80 DEG C of heating water bath, stirring carries Take 1 hour, filter to get filtrate 1.9 liters；Merge to obtain 3.9 liters of extract solutions.Two kinds of extract solutions are mixed into obtain 10.1 liters of extract solutions.
The concentration of two instrument cream with into cream：10.1 liters of extract solutions are added in Rotary Evaporators in batches, 60 DEG C of heating-up temperature, Vacuum 80kPa；2 liters are concentrated into, adds 0.2 kilogram of honey while hot, thick two instrument cream is formed after being sufficiently stirred dissolving.
According to《Chinese Pharmacopoeia 2015 editions》General rule 2341 in Volume Four《Persticide residue determination method》, using gas-chromatography- Tandem mass spectrometry measure wherein pentachloronitrobenzene, total BHC, total DDT, flolimat, parathion-methyl, cypermethrin, 8 kinds of persticide residues such as fenvalerate, cyfloxylate, are not detected.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention. Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability Field technique personnel do not depart from improvement that scope made and modification all should be the present invention's according to the announcement of the present invention Within protection domain.

Claims (10)

  1. A kind of 1. method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent, it is characterised in that comprise the following steps：
    (1) preparation of inorganic adsorbent；
    (2) rare medicinal herbs in herbal paste and common medicinal material are separately extracted, after crushing respectively, adds water, add step (1) described nothing Machine adsorbent, heating, stirring extraction, filtering stay extract solution, the dregs of a decoction are extracted again；
    (3) the rare medicinal herbs extract solution of step (2) is merged with common herbal extract, is placed in low pressure enrichment facility In, heat, concentration, add paste making agent, herbal paste is made.
  2. 2. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 1, it is special Sign is, in the step (1) preparation of inorganic adsorbent specifically use following steps：
    After (1-1) activates ZSM-5 molecular sieve original powder, ZSM-5 molecular sieve activation powder is cooled down to obtain；
    After (1-2) activates magnalium hydrotalcite original powder, magnalium hydrotalcite activation powder is cooled down to obtain；
    ZSM-5 molecular sieve is activated powder by (1-3), magnalium hydrotalcite activation powder mixes, and adds water, activated alumina is used as and bonded Agent, after being sufficiently mixed, extruded moulding, reactivation, it is stored in standby in dry environment.
  3. 3. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 2, it is special Sign is, the silica alumina ratio 5~50 of ZSM-5 molecular sieve, preferably silica alumina ratio 10~25 in the step (1-1).
  4. 4. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 2, it is special Sign is that both ZSM-5 molecular sieve activation powder, magnalium hydrotalcite activation powder mass ratio are (0.1~1) in the step (1-3): (0.1~1), activated alumina quality be ZSM-5 molecular sieve activate powder and magnalium hydrotalcite activate silty amount and 1/5.
  5. 5. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 2, it is special Sign is that ZSM-5 molecular sieve original powder activation condition is 250-450 DEG C in step (1-1), activates more than 1 hour, preferably activates bar Part is：Activated 2~4 hours at 350~400 DEG C of temperature；
    Magnalium hydrotalcite original powder activation condition is 250~400 DEG C in step (1-2), activates more than 1 hour, preferably activation condition For：Activated 2~4 hours at 350~400 DEG C of temperature；
    Step (1-3) extruded moulding post activation condition is 250~400 DEG C and activated more than 1 hour that preferably activation condition is：In temperature Activated 2~4 hours at 350~400 DEG C of degree.
  6. 6. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 1, it is special Sign is that the rare medicinal herbs includes the one or more in ginseng, red ginseng, pseudo-ginseng, ganoderma lucidum；The rare medicinal herbs is crushed to logical Cross 10 mesh standard sieve nets；During the rare medicinal herbs extraction, it is 15 liter/kilogram medicinal materials to add water first, second of addition water For 14 liter/kilogram medicinal materials, add inorganic adsorbent dosage and run after fame the 1/100~1/50 of precious medicinal material quality, water bath heating temperature 60~ 90 DEG C, preferably 70 DEG C, each more than 1 hour heating water bath time, preferably 2~3 hours.
  7. 7. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 1, it is special Sign is that the common medicinal material is other medicinal materials in addition to rare medicinal herbs, and the common medicinal material is crushed to accurate by 10 targets Screen cloth；During the common medicinal material extract, it is 10 liter/kilogram medicinal materials to add water first, and it is 9 liters/kilogram that second, which adds water, Medicinal material, addition inorganic adsorbent dosage are the 1/50~1/20 of common quality of medicinal material, 60~100 DEG C of water bath heating temperature, preferably 80 DEG C, each more than 0.5 hour heating water bath time, preferably 1~2 hour.
  8. 8. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 1, it is special Sign is, the residues of pesticides species of the herbal extract Pesticide Residues thing, wherein inorganic adsorbent energy adsorbing and removing and dense Degree scope includes：0.005~1.0mg/L of pentachloronitrobenzene, total 0.001~0.5mg/L of BHC, total DDT 0.001~ 0.5mg/L, 0.005~1.0mg/L of flolimat, 0.005~1.0mg/L of parathion-methyl, 0.005~1.0mg/ of cypermethrin L, the one or more in 0.005~1.0mg/L of fenvalerate, 0.005~1.0mg/L of cyfloxylate.
  9. 9. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 1, it is special Sign is, the low pressure enrichment facility is the Rotary Evaporators with heater block and vacuum pump part, heating-up temperature 40~80 DEG C, rotavapor under vacuum degree is 60~95kPa；The volume of concentrate is the 1/10~1/5 of extracting liquid volume.
  10. 10. a kind of method that traditional Chinese medical science herbal paste Pesticide Residues are removed using inorganic adsorbent according to claim 1, it is special Sign is that the paste making agent is the one or more in white sugar, xylitol, rock sugar, honey, and paste making agent dosage is every liter of concentrate 0.1~0.3 kilogram of addition paste.
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