CN1994331A - Super micronization method for botanical medicinal, product obtained thereby and use thereof - Google Patents
Super micronization method for botanical medicinal, product obtained thereby and use thereof Download PDFInfo
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Abstract
The invention relates to a method for making stem drug containing xylon and cellulose into ultra micro powder, wherein said method comprises that: mechanically breaking; exploding via steam, treating at low temperature, breaking via airflow, enzyme hydrolyzing via microbe enzyme and extracting and separating. The invention also provides relative product and its application for preparing drug, transferring drug element, etc.
Description
Technical field
The present invention relates to a kind of ultra micro efflorescence method that is used for vegetable drug, or rather, the present invention relates to be used to be rich in the ultra micro efflorescence method of lignocellulose rhizome class vegetable drug, by the application of this method resulting ultra micro efflorescence product and medicine novel formulation under development, extraction and conversion raw material pharmacy effective ingredient, preparation fermented product aspect.
Background technology
Ultra micro efflorescence technology belongs to the material new technical field, is an interdiscipline that is born early 1970s, inter-trade new and high technology, generally is meant the material particles more than the 3mm is crushed to crushing process below the 25 μ m.Material is after ultra micro efflorescence process, become ultrafine powder, because its particulate specific surface area increases, surface energy improves, surface activity strengthens, great changes have taken place with the character at interface in the surface, the physics, the chemical property that cause ultrafine powder usually to demonstrate to be not quite similar with bulk material, and in application, show unique functional characteristic.Constantly perfect along with theory and practice, ultra micro efflorescence technology obtains tremendous development and progress recent decades, at present in all conglomeraties such as oil, chemical industry, mineral products, metallurgy, military project, electronics, medicine, biology and light industrys, and obtained extensive use in the large-tonnage product manufacturing such as food, health product, household chemicals, cosmetics, agricultural product, feedstuff, coating, pottery.
In the process of the modernization of Chinese medicine, ultra micro efflorescence technology also day by day becomes an important new technique, particularly causes extensive concern in the application aspect the prepared slices of Chinese crude drugs form improvement.Decoction pieces is that single medicinal material is after tradition is concocted processing, for the basic medical material of Chinese medicine preparation.As one of main raw material of Chinese medicine type rhizome class plant amedica, its Chinese medicine decoction pieces is to be cut into lamellar, and minority is made coarse powder, for the usefulness of prescription and Chinese medicine preparation production, is the processing first time of tubers Chinese crude drug.Because the Chinese medicine decoction pieces mainly obtains effective ingredient by decocting and/or leaching, dissolution rate is low, waste residue rate height, and many useful pharmacy activity components abandon with medicinal residues, have not only wasted valuable natural resources of Chinese medicinal materials, have also caused environmental pollution.The granule prepared slices of Chinese crude drugs are the processing second time of tubers Chinese crude drug, main method by mechanical activation comminution, after the prepared slices of Chinese crude drugs of tubers plant amedica are ground into the powder of (the about 200-800 μ of particle diameter m) about the 20-80 order, add additive and make graininess, for prescription, Chinese medicine production use.Because its destruction to tubers medicine organizational structure is extremely insufficient, still has dissolution rate problem on the low side.With the oral formulations of its preparation, exist long, the problems such as absorbance is not high, blood drug level instability of dissolve scattered time limit.Begin to adopt the particle diameter of ultra micro efflorescence technology (mainly adopting physical method) acquisition at micron order (1-100 μ m) in recent years, the ultrafine powder prepared slices of Chinese crude drugs of submicron order (0.1-1 μ m), be the processing for the third time of tubers Chinese crude drug, it also is the important breakthrough of carrying out the Chinese crude drug form improvement with Modern Manufacturing Technology, its the most outstanding feature is to have save decoction stripping and/or lixiviate step, the ultrafine powder prepared slices of Chinese crude drugs are directly used in the allotment prescriptions of Chinese medicine, and preparation granule, pill, tablet, oral formulations such as capsule (producing 500 plurality of Chinese granules with these class methods) as Guangdong Yifang Pharmaceutical Co., Ltd, or be used as the raw material that chemical composition of Chinese materia medica extracts.Compare with the Chinese medicine decoction pieces, the ultrafine powder prepared slices of Chinese crude drugs have following outstanding advantage: 1) because the plant cell wall breaking rate significantly increases, the dissolution rate and the absorbance of effective ingredient are significantly increased, thereby can reduce dosage, have saved natural resources of Chinese medicinal materials; 2) after the efflorescence of Chinese crude drug ultra micro, mainly directly prepare oral formulations, not only fully kept pharmacy activity component, and do not have the waste residue generation, reduced the wasting of resources and environmental pollution with the crude drug form; When 3) being used for composition extraction and/or fermentation (biotransformation) acquisition active substance, the yield of pharmacy activity component obviously improves.However, find the present ultrafine powder prepared slices of Chinese crude drugs that obtain with pure physical method in the practice---particularly be rich in the ultrafine powder prepared slices of Chinese crude drugs of lignocellulose rhizome class plant amedica, still have following shortcoming: 1) rhizome is one of medical material position that lignifying is the most outstanding in the medicinal plants, the lignin of most tubers vegetable drugs, hemicellulose and content of cellulose are all above 30% of dry weight, that have even surpass 50%, has bigger hardness and toughness, so in physics ultra micro efflorescence process, than other medical material position (as seed, blade etc.) bigger energy consumption and mechanical loss take place.In addition; a large amount of existence of lignocellulose; make the various organizational structuries and the substructure of plant cell be subjected to indomitable protection; structure iris action to effective ingredient is more obvious; in other words, the separation problem of effective ingredient and irrelevant composition in the not fine solution tubers of the pure physics ultra micro efflorescence technology vegetable drug.2) existing superfine powder metallization processes and follow-up conventional peroral dosage form (tablet, capsule, granule, electuary etc.) granulating process, because the existence of cytoskeletal structures such as lignin and cellulose, making processes raw material has very big dispersibility, can produce bigger dust pollution, can work the mischief to health of operators to a certain extent, also can cause certain environmental pollution.3) ultrafine powder prepared slices of Chinese crude drugs preparation technology only limits to physical pulverization (mainly being machinery and comminution by gas stream) at present, and efficient is not high; Be rich in lignocellulose rhizome class plant amedica, its product process is time consumption and energy consumption especially, contained lignin and cellulosic ratio and state obviously affect the homogeneity of granularity and the quality control of final products, cause production cost higher, thereby patient's drug cost is improved thereupon, and the ability of seeking medical advice and the Chinese medicine that are unfavorable for improving extensive patients are popularized.4) oral formulations that directly prepares of the ultrafine powder prepared slices of Chinese crude drugs, owing to have in the past a large amount of lignins and the cellulose components that should discard with medicinal residues, not only still have the structure iris action to influence dissociating of effective ingredient after taking and absorb, cause liver sausage first pass effect and bioavailability lower, and lignin and the cellulose do not digested and not assimilated by human intestines and stomach also can be by oppositely absorbing moisture, modes such as stimulating gastrointestinal emptying quickening further weaken sticking of stripping pharmacy activity component and absorb, cause the blood drug level instability, thereby have influence on the drug effect performance, finally influenced the therapeutic effect of oral drugs.
Summary of the invention
First purpose of the present invention is to provide the ultra micro efflorescence method of a plant medicinal material, and described vegetable drug is for being rich in lignin, hemicellulose and cellulosic ratio of rhizome medicinal material.Second purpose of the present invention is to provide the ultra micro efflorescence product by the resulting vegetable drug of this ultra micro efflorescence method.The 3rd purpose of the present invention is to provide the purposes of above-mentioned ultra micro efflorescence product.
The ultra micro efflorescence method of vegetable drug provided by the invention comprises the following steps: that quick-fried broken, the deep low temperature procession of mechanical activation comminution, steam, comminution by gas stream, microbial enzyme enzymolysis carry with water and separating.
Above-mentioned vegetable drug is for being rich in lignin, hemicellulose and cellulosic ratio of rhizome medicinal material.
Described mechanical activation comminution is that the tubers vegetable drug is crushed to the fine powder body that particle diameter is 100-200 μ m with physical method.
Described steam explosion is after the mechanical activation comminution product is carried out flash distillation 1-10min with high-pressure water vapor, and the instantaneous recovery atmospheric pressure state forms steam explosion, just because the unexpected adiabatic expansion of internal moisture and by quick-fried broken.
The temperature of above-mentioned water vapour is 180-235 ℃, and pressure is 1.5-2.8Mpa, and flash-off time is 2-3min.
Described deep low temperature procession is with after the suitable drying of the quick-fried broken product of steam, adopts with the liquid nitrogen to be medium or to be the profound hypothermia freezing technology of container with the profound hypothermia refrigerator, and it is carried out freezing processing, material is reached split broken critical point, i.e. glass point.
The temperature of above-mentioned liquid nitrogen is-123 ℃, and the temperature of profound hypothermia refrigerator is-85 ℃.
Described comminution by gas stream is that the deep low temperature procession product is pulverized with the energy breaking method, until obtaining the ultrafine powder that particle diameter is 1-25 μ m.
Above-mentioned energy breaking method is the airflow milling method.
Described microbial enzyme enzymolysis is that the comminution by gas stream product is removed thalline with microorganism after deep fermentation is cultivated fermentation culture is carried out enzyme digestion reaction.
Mentioned microorganism is whiterot fungi whiterot fungi GIM5.178-XW and Trichoderma viride CGMCC3.3711-XW.
It is with the extracting of microbial enzyme enzymolysis product water merceration that described water is proposed separation, and the pharmaceutical chemistry composition of solubility is fully separated with cellulose with insoluble lignin with hemicellulose components, finally obtains needed effective ingredient.
The present invention also provides the ultra micro efflorescence product by the resulting vegetable drug of said method.This ultra micro efflorescence product can be used to prepare Chinese medicine preparation or further extract and/or transform the pharmacy effective ingredient or with the method acquisition fermented product of microbial fermentation, comprise liquid state and/or solid product with physical method, chemical method and/or biological method.
Concrete preparation method is as follows:
1, with after the purification of tubers plant amedica, earlier be cut into traditional decoction pieces with microtome, after suitably dry (water content＜30%), reuse mechanical crushing method (comprise and use ball mill, rod mill, tube mill, and generalized spherical grinding machine vibromill, centrifugal ball milling and planetary mills etc.) is ground into fine powder body (mean diameter 100-250 μ m).
2, it is quick-fried broken obtaining crude drug fine powder body to be implemented steam in steam-explosion jar, carries out flash distillation under high pressure 1.5-2.8MPa, high temperature 180-230 ℃ condition, and decompression suddenly forms steam explosion behind the effect 1-10min, and the material after the processing is bulk to be spongy; Adjust the humidity of material, reach 70-80%.
3, the fine powder body that will finish steam explosion and humidifying places tray, in thermostatic chamber, successively with remove thalline after whiterot fungi GIM5.178-XW fermentation concentrated solution and the fermentation concentrated solution of Trichoderma viride CGMCC3.3711-XW fully mix, under 40 ℃ of constant temperature, carry out enzymolysis, the response time is respectively 12h.
4, after the fine powder body appropriateness drying that enzymolysis is finished, carry out deep-frozen.Method has two: one, with submergence 4-5 time in liquid nitrogen (123 ℃) of enzymolysis powder body, each 2 minutes, powder body is fully freezed to split broken critical point (i.e. " glass point ").The 2nd, place profound hypothermia refrigerator (85 ℃) slowly freezing the enzymolysis powder body, about 60min fully freezes to powder body and splits broken critical point (" glass point ").
5, will be in split broken critical point freeze powder body input air flow pulverizer (comprise use disc type airflow milling, circulation tubular type airflow milling, to spray formula airflow milling, fluid bed to spray formula airflow milling and target formula airflow milling etc.), high-speed impact motion by air-flow is crushed to micron-sized ultrafine powder (mean diameter 1-25 μ m) with material.
6, the ultrafine powder behind the comminution by gas stream adds 5 times sterilized water lixiviate 40 minutes, then lixiviating solution is carried out centrifugal, 3500r/min, 15min separates soluble chemical constituent and insoluble lignin and cellulose.
7, (110 ℃, 98KPa 20min), eliminates assorted bacterium and carries out enzyme-deactivating soluble fraction with high steam.Suitably concentrate, as the raw material that continues extraction, purification or fermentation, or dry (freezing, spraying, vacuum, oven dry) handle, and becomes the ultrafine powder prepared slices of Chinese crude drugs.
Beneficial effect
A kind of new technology path that is rich in lignocellulose tubers plant amedica micronizing that is applicable to provided by the invention.To the plant fiber cells organizational structure on the abundant destructive basis, quick-fried broken in mechanical activation comminution by steam, further eliminate the structure cohesive action of hemicellulose and destroy the grid frame that wooden-cellulose forms, but the enzymatic hydrolyzation of material is obviously improved; By microbial enzyme enzymolysis, obviously reduce lignin and content of cellulose in the fine powder body, destroy its remaining grid frame, further increase the dissolution efficiency of effective ingredient; By the method for deep-frozen repeatedly, increase the rigidity and the brittleness of fine powder body, strengthen its dispersibility, reduce and pulverize time and intensity, thereby energy efficient, reduce and pollute; By further comminution by gas stream, obtain the high-quality ultrafine powder of based on very high purity, granularity equilibrium, interface cleanness; Propose separation by water, distinguish effective ingredient and irrelevant composition, to reach the purpose of final acquisition active constituent content height, infiltration rate is fast, bioavailability is good high-quality oral preparation of Chinese traditional medicinal.
Be fit to use the plant amedica that the method for the invention prepares the ultrafine powder prepared slices of Chinese crude drugs, it is selected according to there being two: 1. tubers plant amedica; 2. lignin, hemicellulose and content of cellulose surpass 20% of dry weight in the structure.Comprise: Radix Glycyrrhizae, Radix Ginseng, Radix Bupleuri, Radix Platycodonis, Radix Polygalae; Further, also comprise Radix Notoginseng, Rhizoma Smilacis Glabrae, Radix Et Rhizoma Rhei, Rhizoma Dioscoreae, Rhizoma Chuanxiong, river bone, Radix Salviae Miltiorrhizae, Rhizoma Cimicifugae, Rhizoma Gastrodiae, Radix Asparagi, the Radix Aucklandiae, Radix Achyranthis Bidentatae, Rhizoma Zingiberis Recens, the Rhizoma Atractylodis Macrocephalae, the Pseudobulbus Bletillae (Rhizoma Bletillae), Herba Dendrobii, Cortex Lycii, Radix Polygoni Multiflori, Radix Adenophorae (Radix Glehniae), Radix Paeoniae, Radix Stephaniae Tetrandrae, the Rhizoma Anemarrhenae, Rhizoma Polygoni Cuspidati, Radix Peucedani, Radix Sophorae Flavescentis, the Radix Linderae, Poria, Radix Rehmanniae, Cortex Phellodendri, Radix Scutellariae, the Radix Astragali, Rhizoma Coptidis, Rhizoma Polygonati, Radix Puerariae, Rhizoma Alismatis, Radix Angelicae Pubescentis, Polyporus, Radix Sophorae Tonkinensis, Radix Isatidis; Further, also comprise Rohdea japonica Roth, Radix Rumicis Japonici dish, Radix Gentianae, panax japonicus, Radix Et Rhizoma Nardostachyos, Radix Rubiae, Rhizoma Acori Graminei, Radix Curcumae, the Radix Angelicae Dahuricae, Rhizoma Corydalis, Rhizoma Atractylodis, Bulbus Fritillariae Uninbracteatae, the Radix Stemonae.
The ultrafine powder prepared slices of Chinese crude drugs involved in the present invention are compared with the ultrafine powder prepared slices of Chinese crude drugs that obtained with physical method (machinery or comminution by gas stream) merely at present, have following beneficial effect:
1, the mechanical crushing method (the present invention adopts the ball mill pulverizing method) that is used for the tubers plant amedica involved in the present invention, only need the Chinese medicine decoction pieces of intensive drying (humidity＜30%) is ground into fast the fine powder body of mean diameter 100-250 μ m (60-200 order), not high to particulate uniformity requirement.Weak point consuming time, energy consumption is low, and dust is few, and is little to staff and environmental hazard; All can use as long as be suitable for pulverizing the mechanical crushing method and the equipment that are rich in lignocellulosic material, so universality and good economy performance.
2, the quick-fried broken method of steam that is used for the tubers plant amedica involved in the present invention, the mechanical damage effect that external force depolymerisation and instant decompression steam explosion by the High Temperature High Pressure flash distillation spurts makes the softening and part depolymerization of lignin in the crude drug fine powder body that is rich in lignocellulose; Hemicellulose fully exposes and is degraded into soluble sugar rapidly; The bonding strength of cellulose net lattice structure is weakened greatly, and cell wall is broken in a large number, and inner surface fully exposes, and specific surface area increases, but enzymatic hydrolyzation obviously improves; Its resultant effect makes that lignin and cellulosic dissociating property improve greatly in the raw material.Simultaneously, the instantaneity of flash distillation and steam explosion has also guaranteed that bioactive ingredients is not obviously destroyed in the raw material.
3, the enzyme hydrolysis process that is used for tubers plant amedica fine powder body involved in the present invention, system is with the fermentation concentrated solution of the Trichoderma viride (the present invention CGMCC3.3711-XW) of the white rot fungi (the present invention GIM5.178-XW) that contains the main enzyme of lignin degrading system and high yield hemicellulase, cellulase, and the timing enzymolysis is finished on the tray in thermostatic chamber.By the enzyme hydrolysis on the quick-fried broken basis of steam, the lignin in the material, hemicellulose, cellulose are further degraded, and the lignocellulose structure is further destroyed, and the inside and outside composition of cell is further dissociated, and effectively bioactive substance is discharged more fully.Simultaneously, the hemicellulose that is degraded and part lignin, cellulose become benefit materials such as monosaccharide, disaccharide, oligosaccharide and polysaccharide soluble, that can be absorbed by the body and/or utilize.
4, the deep-frozen method that is used for the tubers plant amedica involved in the present invention is the ultra micro efflorescence processing that the sharp freezing technology is applied to the tubers plant amedica.According to material characteristic; with the superfine powder sharp freezing of enzymolysis to splitting broken critical point (" glass point "); increase its dispersibility and fragility; for follow-up energy is pulverized simplification preparation technology; shorten running time; save the cooling energy consumption, particularly obviously help reducing the bioactive ingredients in equipment loss and the protection raw material.
5, the energy breaking method (the present invention adopts the high velocity air breaking method) that is used to be rich in lignocellulose tubers plant amedica involved in the present invention, system combines the energy crushing technology with the sharp freezing technology new technology, promptly sharp freezing to the crude drug fine powder body that splits broken critical point is sent in the jet mill, will be freezed the ultrafine powder that material is ground into mean diameter 1-25 μ m (500-12500 order) rapidly by the high-speed impact of air-flow.With conventional gas flow crushing process relatively, new technology has weak point consuming time, energy consumption is low, the purity height, interface cleanness, equipment loss is little, is easy to produce in enormous quantities and can effectively protects in the raw material advantages such as bioactive ingredients.
6, the ultra micro efflorescence method products therefrom that the present invention relates to---be rich in the beneficial effect of the ultrafine powder prepared slices of Chinese crude drugs of lignocellulose tubers plant amedica in application facet:
When 1) being used for directly preparing oral preparation of Chinese traditional medicinal, at first, because above-mentioned ultra micro efflorescence method, lignocellulose compositions a large amount of in the raw material are degraded, it dissociates from raw material to effective ingredient and the structure iris action of stripping is obviously eliminated, with the ultrafine powder prepared slices of Chinese crude drugs of traditional decoction pieces of equivalent, the granule prepared slices of Chinese crude drugs and the preparation of simple mechanical method relatively, the dissolution rate of effective ingredient improves (seeing embodiment 1) greatly, means that promptly curative effect improves; Secondly, the increase of effective ingredient reduces the waste residue generation rate, has not only reduced pollution, and raw material availability obviously improves, and has saved raw material resources, and the minimizing of irrelevant composition also means the minimizing of side effect; Once more, highly decomposing makes effective ingredient be able to be present in dispersant or the excipient with molecule, colloid or microcrystalline state, the medicine total surface area increases, dissolving and infiltration rate are accelerated, abundant dissociated active component has bipolarity from raw material, make it be more conducive to intestinal and stick and absorb, thereby improved bioavailability, can bring into play efficient, quick-acting effects.
When 2) being used for extraction or purification effective ingredient, because aforementioned processing has increased the dissolution rate of raw material of Chinese medicine effective ingredient greatly, and the structure iris action that has fully destroyed lignocellulose, so can make further separation, extraction process and step become simple, cost reduces, the yield of effective ingredient and purity all can significantly improve (seeing embodiment 2), thereby further strengthen the curative effect and the benefit of raw material Chinese medicine.
When 3) generating new drug as the fermentation substrate biotransformation, with mechanical activation comminution ultrafine powder tunning relatively, the present invention can make that effective ingredient very obviously increases (seeing embodiment 3) in the raw material of Chinese medicine.
Description of drawings
Fig. 1 is a vegetable drug ultra micro efflorescence flow chart of the present invention.
The specific embodiment
Embodiment 1: the present invention is to the influence of the dissolution rate of the total Saponin of Radix Bupleuri
The different disposal method is carried out by the following method to the comparative experiments of the total Saponin stripping of Radix Bupleuri content influence in the crude drug Radix Bupleuri:
At first Radix Bupleuri is done following processing: after Radix Bupleuri was purified, microtome was cut into traditional decoction pieces, and suitably dry back reuse ball mill is ground into fine powder body (mean diameter 100-250 μ m); Obtaining crude drug fine powder body is implemented steam in steam-explosion jar quick-fried broken (at high pressure 2.2MPa, carry out flash distillation under 180 ℃ the condition, decompression suddenly forms steam explosion behind the effect 5min), the material after the processing is bulk to be spongy, the humidity of the whole material of the step of going forward side by side reaches 70-80%; The Radix Bupleuri superfine powder of finishing humidifying is placed tray, in thermostatic chamber, successively with remove thalline after whiterot fungi GIM5.178-XW fermentation concentrated solution and the fermentation concentrated solution of Trichoderma viride CGMCC3.3711-XW fully mix, under 40 ℃ of constant temperature, carry out enzymolysis, the response time is respectively 12h; After the fine powder body appropriateness drying that enzymolysis is finished,, each 2 minutes, powder body is fully freezed to split broken critical point (i.e. " glass point ") the submergence 4 times in liquid nitrogen (123 ℃) of enzymolysis powder body; To be in split broken critical point freeze powder body input air flow pulverizer, be crushed to micron-sized ultrafine powder (mean diameter 1-25 μ m), obtain Radix Bupleuri micropowder body behind the enzymolysis.
Each step in processing procedure, accurately take by weighing each 1000g of ultrafine powder behind ultrafine powder behind Radix Bupleuri tradition decoction pieces (2 parts), granule decoction pieces, ultramicro decoction piece (only physical pulverization), the steam explosion, the enzymolysis respectively, adopt thin layer chromatography to measure the total Saponin of Radix Bupleuri, the method that detection method was stipulated in the version with reference to the Pharmacopoeia of the People's Republic of China in 2005 is carried out, and more different crude drug processing methods are to the influence of the total Saponin stripping of Radix Bupleuri content.
Different crude drug processing methods are to the influence/g1000g of the total Saponin stripping of Radix Bupleuri content
-1
| Processing method | Radix Bupleuri total saponin content x | Meansigma methods | ||
| The tradition decoction pieces decocts traditional decoction pieces merceration granule decoction pieces merceration ultramicro decoction piece merceration steam explosion microbody merceration enzymolysis microbody merceration | 31.933 23.436 32.647 54.375 68.901 104.235 | 32.401 22.941 33.301 56.213 67.438 100.584 | 32.578 23.182 33.251 55.972 69.943 104.317 | 32.455 23.387 33.417 56.038 69.905 102.953 |
Embodiment 2: the extraction ratio of Radix Puerariae total flavones (extracting relatively with the immersion of Radix Puerariae alcohol, Radix Puerariae infusion) different disposal method is carried out by the following method to the comparative experiments of Radix Puerariae total flavones stripping content influence in the crude drug Radix Puerariae:
To be cut into traditional decoction pieces after the Radix Puerariae purification, dry back reuse ball mill is ground into fine powder body (mean diameter 100-250 μ m), it is quick-fried broken (at high pressure 2.2MPa to implement steam again in steam-explosion jar, carry out flash distillation under 180 ℃ the condition, decompression suddenly forms steam explosion behind the effect 5min), material after the processing is bulk to be spongy, and adjusts humidity of materials, reaches 70-80%; Powder of Radix Puerariae after further gas exposes to the sun places tray, with successively with remove thalline after whiterot fungi GIM5.178-XW fermentation concentrated solution and the fermentation concentrated solution of Trichoderma viride CGMCC3.3711-XW fully mix, carry out enzymolysis under 40 ℃ of constant temperature, the response time is respectively 12h; After the raw material appropriateness drying that enzymolysis is finished, submergence is 4 times in liquid nitrogen (123 ℃), and each 2 minutes, powder body is fully freezed to split broken critical point, input air flow pulverizer then, acquisition is crushed to micron-sized Radix Puerariae ultrafine powder (mean diameter 1-25 μ m).Each step in processing procedure, accurately take by weighing ultrafine powder behind Radix Puerariae tradition decoction pieces (2 parts), granule decoction pieces, ultramicro decoction piece (only physical pulverization), the steam explosion, enzymolysis respectively after each 1000g of ultrafine powder be equipped with inspection.
Be contrast with the puerarin standard substance then, adopt ultraviolet spectrophotometry to measure Radix Puerariae total flavones, concrete grammar is: accurately take by weighing 0.5g Radix Puerariae powder (crossing 80 mesh sieves), add 70% alcoholic solution 100ml, put into cable-styled extractor.Extracted 8 hours down at 85 ℃, filter with vacuum pump, collect filtrate, evaporate to dryness on Rotary Evaporators with 95% ethanol standardize solution, detects by the formulating method of standard curve, records that general flavone content is 7.68% in the Herba Gelsemii Elegantis.Adopting 70% concentration of alcohol, 7 times quantity of solvent, 2 hours extraction time and extraction time subsequently is 4 unified detection methods, respectively ultrafine powder behind ultrafine powder and the enzymolysis behind Radix Puerariae tradition decoction pieces, granule decoction pieces, ultramicro decoction piece (only physical pulverization), the steam explosion is calculated its extraction ratio.
Different crude drug processing methods are to the influence (%) of Radix Puerariae total flavones extraction ratio
| Processing method | Radix Puerariae total flavones extraction ratio (%) | Meansigma methods (%) | ||
| Ultrafine powder behind the ultrafine powder enzymolysis behind the Radix Puerariae tradition decoction pieces granule decoction pieces ultramicro decoction piece steam explosion | 85.3 87.2 92.9 91.2 94.5 | 83.9 90.7 91.4 95.1 96.2 | 86.1 89.3 94.2 93.1 96.7 | 85.1 89.1 92.8 93.1 95.8 |
Embodiment 3: glycyrrhizic acid fermentation back enoxolone conversion ratio (comparing with the fermentation of physical pulverization ultrafine powder) different disposal method is divided three steps to the comparative experiments that influences of glycyrrhizic acid fermentation back enoxolone conversion ratio: at first Radix Glycyrrhizae is carried out pre-treatment and obtain test sample, secondly test sample is fermented, detect glycyrrhizic acid and enoxolone with the high performance liquid chromatogram method at last, calculate conversion ratio.
To be cut into traditional decoction pieces after the Radix Glycyrrhizae purification, dry, the reuse ball mill is ground into fine powder body (mean diameter 100-250 μ m), it is quick-fried broken (at high pressure 2.2MPa to implement steam again in steam-explosion jar, carry out flash distillation under 180 ℃ the condition, decompression suddenly forms steam explosion behind the effect 5min), and adjust humidity of materials, reach 70-80%; Radix Glycyrrhizae powder after further gas exposed to the sun places tray, successively with remove thalline after whiterot fungi GIM5.178-XW and Trichoderma viride CGMCC3.3711-XW fermentation concentrated solution fully mix, 40 ℃ of constant temperature enzymolysis, the response time is respectively 12h; After the raw material appropriateness drying that enzymolysis is finished, submergence is 4 times in liquid nitrogen (123 ℃), and each 2 minutes, input air flow pulverizer then, acquisition is crushed to micron-sized Radix Glycyrrhizae ultrafine powder (mean diameter 1-25 μ m).In processing procedure, accurately take by weighing ultramicro decoction piece (only physical pulverization), enzymolysis respectively after each 1000g of ultrafine powder standby.
To the powder body sample behind ultramicro decoction piece and the enzymolysis, with at least a lactobacillus ferment that contains glycuronidase, a strain of Lactobacillus (Lactobacillus) for example, anaerobic environment, stirs the fermentation liquid that obtains behind the fermentation 18h by 37 ℃.Except using a kind of lactobacillus ferment at least, also can be undertaken by other microorganism that contains glycuronidase.The method that the detection method of glycyrrhizic acid and enoxolone was stipulated in the version with reference to the Pharmacopoeia of the People's Republic of China in 2005 detects, according to the high-efficient liquid phase chromatogram technique measuring glycyrrhizic acid and the enoxolone of pharmacopeia regulation, compare of the influence of two kinds of different crude drug processing methods to the enoxolone conversion ratio.
Different crude drug processing methods are to the influence (%) of enoxolone conversion ratio
| Processing method | Enoxolone conversion ratio (%) | Meansigma methods | ||
| Physical pulverization enzymolysis powder body | 81.3 95.2 | 80.1 96.7 | 84.9 94.8 | 82.1 95.6 |
Claims (17)
1, the ultra micro efflorescence method of vegetable drug comprises the following steps: that quick-fried broken, the deep low temperature procession of mechanical activation comminution, steam, comminution by gas stream, microbial enzyme enzymolysis carry with water and separating.
2, method according to claim 1, wherein said vegetable drug are ratio of rhizome medicinal material.
3, method according to claim 2, wherein said ratio of rhizome medicinal material is for being rich in lignin, hemicellulose and cellulosic ratio of rhizome medicinal material.
4, method according to claim 1, wherein said mechanical activation comminution are that described medical material is pulverized with the method for physics, until obtaining the fine powder body that particle diameter is 100-200 μ m.
5, method according to claim 1, wherein said steam quick-fried broken be after the mechanical activation comminution product is carried out flash distillation 1-10min with high-pressure water vapor, the instantaneous recovery atmospheric pressure state forms steam explosion, just because the unexpected adiabatic expansion of internal moisture and by quick-fried broken.
6, method according to claim 5, the temperature of wherein said water vapour are 180-235 ℃, and pressure is 1.5-2.8Mpa, and flash-off time is 2-3min.
7, method according to claim 1, wherein said deep low temperature procession is with after the suitable drying of the quick-fried broken product of steam, adopts with the liquid nitrogen to be medium or to be the profound hypothermia freezing technology of container with the profound hypothermia refrigerator, and it is carried out freezing processing, material is reached split broken critical point, i.e. glass point.
8, method according to claim 7, the temperature of wherein said liquid nitrogen are-123 ℃, and the temperature of described profound hypothermia refrigerator is-85 ℃.
9, method according to claim 1, wherein said comminution by gas stream are that the method that the deep low temperature procession product is pulverized with energy is pulverized, until obtaining the ultrafine powder that particle diameter is 1-25 μ m.
10, method according to claim 9, wherein said energy breaking method is the airflow milling method.
11, method according to claim 1, wherein said microbial enzyme enzymolysis are that the comminution by gas stream product is removed thalline with microorganism after deep fermentation is cultivated fermentation culture is carried out enzyme digestion reaction.
12, method according to claim 11, wherein said microorganism are whiterot fungi GIM5.178-XW and Trichoderma viride CGMCC3.3711-XW.
13, method according to claim 1, it is with the extracting of microbial enzyme enzymolysis product water merceration that wherein said water is proposed separation, the pharmaceutical chemistry composition of solubility is fully separated with cellulose with insoluble lignin with hemicellulose components, finally obtain needed effective ingredient.
14, by the ultra micro efflorescence product of the resulting vegetable drug of the described method of claim 1.
15, the purposes of the ultra micro efflorescence product of the described vegetable drug of claim 14 is used to prepare Chinese medicine preparation.
16, the purposes of the ultra micro efflorescence product of the vegetable drug of claim 14 is used for physical method, chemical method and/or biological method and further extracts and/or transform the pharmacy effective ingredient.
17, the purposes of the ultra micro efflorescence product of the vegetable drug of claim 14, the method that is used for microbial fermentation obtains fermented product, comprises liquid state and/or solid product.
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