CN103520030A - Preparation method of Chinese herbal compound with natural anti-corrosion effect - Google Patents
Preparation method of Chinese herbal compound with natural anti-corrosion effect Download PDFInfo
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Abstract
A preparation method of a Chinese herbal compound with a natural anti-corrosion effect comprises the steps as follows: (1), pulverizing muskroot-like semiaquilegia roots and herba violae into coarse powder through a pulverizer; (2), adding a solvent to the coarse powder and grinding the coarse powder into suspension of fine powder through a colloid mill; (3), putting flos chrysanthemi indici, honeysuckle, dandelion and selfheal in an extracting tank, and adding the suspension of the fine powder in the last step for normal temperature circulation extraction; and (4), performing conventional sedimentation and filtration treatment. By means of the preparation method, the problems of low transfer rate of effective constituents, multiple dissolved impurities, dark color, many steps, long operating period, high cost and the like of traditional Chinese medicine preparation technologies can be solved.
Description
Technical field
The present invention relates to a kind of preparation method of extracting solution, more particularly, relate to a kind of have natural anticorrosion effect Chinese medicine compound preparation method.
Background technology
At present the most frequently used method of Chinese drug preparation be that decocting boils, concentrate, the technique such as precipitate with ethanol, concentrated, filtration, it is few that the standby lower boiling composition of extracting solution of this legal system retains, impurity stripping is many, color is dark, affects its interpolation use in cosmetics finished product.And whole processing step is loaded down with trivial details, and the production cycle is long, the equipment needing is many, and energy consumption is large, and production cost is higher, and ethanol consumption is large.
In order to reduce the stripping of macromole pigment and to retain low boiling point component, also useful cold percolation technique, but this method solvent load causes greatly follow-up concentrated amount large, and the leaching process time is long, and generally medical material is carried out to coarse powder, and leaching process easily stops up.
Adding use in cosmetics to is an important directions of plant extract industry development, there is the very large market space, how to prepare meet cosmetics add to require be high concentration again light-colored extracting solution be current urgent problem, utilize material diffusion feature, operating feature in conjunction with existing device is carried out rational modification, optimization and combination, is the feasible thinking addressing this problem.
Summary of the invention
It is dark that technical problem to be solved by this invention has been to overcome Chinese medicine extraction liquid color prepared by traditional preparation technology, effective ingredient retains few, impurity is many, complex steps, production cycle is long, energy consumption is large, the problems such as ethanol consumption is large, according to the diffusion property of medical material, the medical material that is not easy to be permeated by solvent is prepared into fine powder suspension by colloid mill, go circulatory displacement to extract the medical material easily being permeated by solvent, reduce the stripping of pigment, better retain micromolecule and low-boiling point material, leaching process does not produce clogging, significantly reduce the consumption of solvent, save concentrated, the steps such as wine is heavy, reach simplification processing step, shorten the production cycle, the effect of minimizing energy consumption etc., meet cosmetics instructions for use and cost-saving on have significant contribution.
Concrete steps:
(1) Radix Semiaquilegiae and Herba Violae are pulverized with pulverizer, be ground into 20 ~ 40 order coarse powder;
(2) coarse powder is added to water, or the alcoholic solution of low 75 degree, quantity of solvent is 2 ~ 4 times, wears into the suspension of 2 ~ 50 μ m fine powders with colloid mill;
(3) pack Flos Chrysanthemi Indici, Flos Lonicerae, Herba Taraxaci, Spica Prunellae 4 into extraction pot for medical material, the suspension that adds the fine powder in back, carrying out room temperature circulation extracts, extract 0 ~ 30 ℃ of temperature, for volume 2.5L extraction pot, its circulation rate is 1 ~ 10L/h, and the extraction pot of other volumes changes uninterrupted with the equal principle of linear velocity, and extraction time is 2 ~ 6h.
(4) sedimentation is spent the night, and gets supernatant liquid filtering.
Positive effect of the present invention:
(1) the present invention overcomes the shortcoming of traditional decoction method, utilizes extract at low temperature to reduce the stripping of the macromole pigments such as chlorophyll, and strengthens the reservation to low-boiling point material, and the extracting solution color of preparation is more shallow, meets cosmetics instructions for use;
(2) with the medical material easily being permeated by solvent, directly in percolate pot, extract, avoided leaching process obstruction, handled easily;
(3) medical material of dense structure is worn into fine powder suspension with colloid mill, in leaching process, directly through the medical material layer of percolate pot, participate in circulation, both increased the stripping of medical material effective ingredient, the clogging of avoiding again coarse powder filler to produce;
(4) by wear into fine powder suspension with colloid mill, directly extract other medical materials, and use circulatory displacement mode, significantly reduce the use of solvent, improve the content of effective ingredient in extracting solution, shorten the time of leaching process, reduce the follow-up step such as concentrated, significantly simplified technique, shorten the production cycle;
(5) the present invention be according to the diffusion property of material to extracting medical material, carry out differentiating and processing, as long as existing equipment is done to less improvement and combination can realize the method, make to extract easy to operate, effective ingredient is retained, of light color;
(6) energy efficient: the operating unit of energy consumption maximum is upgrading unit, and this case saves that traditional handicraft 2 times is concentrated, wine is heavy and the energy consumption of cold preservation step, has greatly reduced energy consumption;
(7) safety: can reduce and even not use the organic solvents such as ethanol, production process is safer.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the circulatory displacement device of invention.
The specific embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.
Embodiment 1:
Technological process:
Circulatory displacement device and technological process as shown in Figure 1.Circulatory displacement device is connected by percolate pot 1, pump 2, effusion meter 3, heating/cooling device 4 and valve 5, forms circulating device.The medical material easily being permeated by solvent packs in percolate pot 1, the medical material that is difficult for being permeated by solvent is first pulverized with pulverizer, then reinstate with solvent one suspension that colloid mill is further ground into fine powder, add in percolate pot 1 again and mix with other medical materials, in percolate pot 1, pump 2 and heating/cooling device 4, circulation is extracted afterwards.
Bacteriostatic test step:
(1) test strain
Staphylococcus aureus (ATCC8739), escherichia coli (ATCC6538), bacillus pyocyaneus (ATCC9027), candida albicans (ATCC10231), Aspergillus niger (ATCC16404).
(2) culture medium
TSB solid medium: peptone 10g/L, NaCl10g/L, K2HPO42.5g/L, yeast extract 3g/L, agar 15g/L, distilled water dissolves, and regulating pH is 7.2 ± 0.2,115 ℃ of autoclaving 20min; TSB fluid medium: peptone 10g/L, NaCl10g/L, K2HPO42.5g/L, yeast extract 3g/L, distilled water dissolves, and regulating pH is 7.2 ± 0.2,115 ℃ of autoclaving 20min;
SDB solid medium: peptone 10g/L, glucose 20g/L, K2HPO43g/L, yeast extract 5g/L, agar 15g/L, distilled water dissolves, 115 ℃ of autoclaving 20min; SDB fluid medium: peptone 10g/L, glucose 20g/L, K2HPO43g/L, yeast extract 5g/L, distilled water dissolves, 115 ℃ of autoclaving 20min.
(3) collecting cells and inoculation
Get the staphylococcus aureus of glycerol preservation, escherichia coli, bacillus pyocyaneus 100 μ L coat on TSB solid medium, cultivate 2d for 37 ℃, resuspended with normal saline, obtain bacteria suspension, and with plating method counting, test bacteria concentration are adjusted into 10
5～10
6cFU/mL.
Candida albicans and Aspergillus niger 100 μ L coat on SDB solid medium, cultivate 2d for 30 ℃, resuspended with normal saline, obtain bacteria suspension, and with plating method counting, test bacteria concentration are adjusted into 10
5～10
6.
(4) mensuration of sample bacteriostasis
Cylinder plate method
In culture dish, pour TSB or SDB solid medium into, after solidifying, in this culture medium, evenly bacterium 100 μ L are tested in coating.Equidistant 2 aseptic Oxford cups [internal diameter (6.0 ± 0.1) mm of putting in culture medium, external diameter (8.0 ± 0.1) mm, high (10.0 ± 0.1) mm injects respectively 200 μ L testing samples in cup, with normal saline or containing the normal saline of a certain amount of DMSO in contrast.In 37 ℃ or 30 ℃ of calorstats, cultivate after 2d, with ruler, measure the antibacterial circle diameter of various medicines, get its meansigma methods.
Microdilution plate method
In micropore, add 100 μ L testing samples (initial concentration), then add containing test bacteria concentration 1.0 * 10
5cFU/mL is 2 * TSB or 2 * SDB fluid medium, 100 μ L, mixes, and the test concentrations of testing sample is initial concentration 50%.In 30 ℃ or 37 ℃ of calorstats, cultivate after 2d, observe and have asepsis growth.The prerequisite of result judgement is that growth control is good, and blank asepsis growth is clear.
(5) mensuration of minimum inhibitory concentration (MIC value)
1. the assay method of minimum inhibition staphylococcus aureus concentration (MIC), minimum inhibition e. coli concentration (MIC), minimum inhibition bacillus pyocyaneus concentration (MIC), minimum inhibition candida albicans concentration (MIC) is as follows:
(1) medicinal liquid preparation
Testing sample is become to experimental concentration with normal saline dilution.
(2) 2 * TSB or 2 * SDB fluid medium dilution bacteria suspension for bacterium solution preparation, making its final bacteria concentration is l0
5cFU/mL.
(3) cultivate and result interpretation adds bacterium liquid 100 μ L and medicinal liquid 100 μ L in micropore, establish the normal growth that does not add the negative control of bacterium and do not add medicinal liquid simultaneously and contrast, every kind of medicine do 3 parallel, average.Put 37 ℃ or 30 ℃ of wet boxes and hatch, observed result after 48h, adopts direct method reading out data.The prerequisite of result judgement is that growth control is good, and blank asepsis growth is clear, and with the rising of drug level gradient, the growth of bacterium is suppressed in other hole.
2. minimum inhibition aspergillus niger concentration (MIC) is measured
Adopt cylinder plate method, in culture dish, pour SDB solid medium into, after solidifying, in this culture medium, add Aspergillus niger (10
5cFU/ml) 100 μ L, evenly coating.Equidistantly in culture medium put 3 aseptic Oxford cups [high (10.0 ± 0.1) mm injects respectively the sample (with normal saline dilution) of 200 μ L variable concentrations in cup for internal diameter (6.0 ± 0.1) mm, external diameter (8.0 ± 0.1) mm.Establish the normal growth contrast and the normal saline contrast that do not add specimen simultaneously.The prerequisite of result judgement is growth control and normal saline contrast well-grown, and with the rising of drug level gradient, the growth of bacterium is suppressed for other.
Extraction step:
(1) to each 50 grams of Radix Semiaquilegiae and Herba Violaes, with pulverizer, pulverize, be ground into 20 ~ 40 order coarse powder;
(2) coarse powder is added to 2L water, with colloid mill, wear into the suspension of 2 ~ 50 μ m fine powders;
(3) Flos Chrysanthemi Indici 150g, Flos Lonicerae 150g, Herba Taraxaci 50g, Spica Prunellae 50g are packed in the extraction pot of 2.5L, add the extraction that circulates of the suspension of the fine powder in back, extract 30 ℃ of temperature, circulation rate is 10L/h, and extraction time is 6h.
(4) sedimentation is spent the night, and gets supernatant liquid filtering, and moisturizing, to 1.5L, obtains.
Embodiment 2:
(1) each 50 grams of Radix Semiaquilegiae and Herba Violaes are pulverized with pulverizer, be ground into 20 ~ 40 order coarse powder;
(2) coarse powder is added to 1.5L40% alcoholic solution, with colloid mill, wear into the suspension of 2 ~ 50 μ m fine powders;
(3) Flos Chrysanthemi Indici 150g, Flos Lonicerae 150g, Herba Taraxaci 50g, Spica Prunellae 50g are packed in 2.5L extraction pot, add the extraction that circulates of the suspension of the fine powder in back, extract 15 ℃ of temperature, circulation rate is 5L/h, and extraction time is 4h.
(4) sedimentation is spent the night, and gets supernatant liquid filtering, and moisturizing, to 1.5L, obtains.
Embodiment 3:
(1) Radix Semiaquilegiae and Herba Violae are pulverized with pulverizer, be ground into 20 ~ 40 order coarse powder;
(2) coarse powder is added to 1L75% alcoholic solution, with colloid mill, wear into the suspension of 2 ~ 50 μ m fine powders;
(3) Flos Chrysanthemi Indici 150g, Flos Lonicerae 150g, Herba Taraxaci 50g, Spica Prunellae 50g are packed in 2.5L extraction pot, add the extraction that circulates of the suspension of the fine powder in back, extract 0 ℃ of temperature, circulation rate is 1L/h, and extraction time is 2h.
(4) sedimentation is spent the night, and gets supernatant liquid filtering, and moisturizing, to 1.5L, obtains.
Comparative example 1:
Traditional decoction method:
(1) Flos Chrysanthemi Indici 150g, Flos Lonicerae 150g, Herba Taraxaci 50g, Spica Prunellae 50g, Radix Semiaquilegiae 50g, Herba Violae 50g, pack 5L round-bottomed flask into, adds the alcoholic solution of 3L40%, to heating and refluxing extraction 2h in electric jacket;
(2) filter, repeat to extract 1 time;
(3) filter, merging filtrate, is concentrated into proportion (55 ℃ of surveys) 1.1;
(4) add 95% ethanol alcohol to be sink to 75%, cold preservation is spent the night;
(5) get supernatant liquid filtering, be concentrated into 1.5L.
Comparative example 2:
Tradition percolation:
(1) Flos Chrysanthemi Indici 150g, Flos Lonicerae 150g, Herba Taraxaci 50g, Spica Prunellae 50g, Radix Semiaquilegiae 50g, Herba Violae 50g, break into 20 ~ 40 order coarse powder with pulverizer after mixing;
(2) use the alcohol solution dipping 8h of 1L40%;
(3) pack 2.5L percolate pot into, with 0.5mlmin
-1kg
-1speed is carried out percolation, and percolation volume is 7.5L;
(4) filter extracting solution, be concentrated into 1.5L.
The present invention compares with traditional mode of production, and in process, indices is as shown in table 1:
Table 1
As shown in Table 1, the present invention program obviously shortens the production cycle, and solvent load significantly reduces, and color is more shallow, and fungistatic effect is better than traditional handicraft, and this may be because whole process is without high-temperature operation, and antipathogenic composition is retained better.
In the present invention, as apply the extraction pot of other volumes, can change flow with the equal principle of linear velocity.
Technology of the present invention is equally applicable to retain the preparation of the Chinese medicine extraction liquid of micromolecule, low boiling point component.
Should be understood that, % of the present invention and wt% all refer to quality percentage composition.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (5)
1. have natural anticorrosion effect Chinese medicine compound a preparation method, it is characterized in that, raw material is adopted to following concrete preparation process:
(1) Radix Semiaquilegiae and Herba Violae are broken into 20 ~ 40 order coarse powder with pulverizer;
(2) coarse powder step (1) being made adds the suspension that is milled into 2 ~ 50 μ m fine powders after solvent with colloid mill;
(3) pack Flos Chrysanthemi Indici, Flos Lonicerae, Herba Taraxaci, Spica Prunellae 4 taste medical materials into extraction pot, add the fine powder suspension in described step (2), carry out 0 ~ 30 ℃ of circulation and extract.
2. preparation method as claimed in claim 1, is characterized in that, the constituent mass proportioning of described raw material is: 30 parts of Spica Prunellaes, 30 parts of Flos Loniceraes, 10 parts of Flos Chrysanthemi Indicis, 10 parts of Herba Taraxacis, 10 parts of Radix Semiaquilegiaes, 10 parts of Herba Violaes.
3. preparation method as claimed in claim 1, it is characterized in that, colloid mill in circulation extraction in described step (3) and step (2) solvent adopting of milling is the alcoholic solution that concentration is less than 75wt%, the medical material that is specially dense structure is first made suspension with colloid mill, add again the medical material of outer circulating extracting Guan Dui tissue looseness to extract, extract 0 ~ 30 ℃ of temperature, extraction time is 2 ~ 6h, and the liquid circulation velocity numerical value of described extraction pot is 0.4-4 times of extraction pot volume numerical value.
4. preparation method as claimed in claim 3, is characterized in that, described extraction pot for volume be 2.5L extraction pot, its liquid circulation velocity is 1 ~ 10L/h, the extraction pot of other volumes changes flow and rotating speed size with the equal principle of linear velocity.
5. preparation method as claimed in claim 1, is characterized in that, described extraction equipment used can carry out circulatory displacement.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103830138A (en) * | 2014-02-17 | 2014-06-04 | 完美（中国）有限公司 | Natural plant compound having preservative effect and daily health product |
| CN104351329A (en) * | 2014-11-13 | 2015-02-18 | 山东商业职业技术学院 | Composite leaching vegetable fresh-keeping agent for tragus berteronianus and preparation method of fresh-keeping agent |
| CN107823023A (en) * | 2017-12-21 | 2018-03-23 | 李冬梅 | A kind of natural plant extracts composition and its application in cosmetics |
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Patent Citations (4)
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| CN101249315A (en) * | 2007-11-26 | 2008-08-27 | 中山装备制造工业研究院 | Method for normal temperature high voltage continuous extracting natural product effective ingredient and equipment thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103830138A (en) * | 2014-02-17 | 2014-06-04 | 完美（中国）有限公司 | Natural plant compound having preservative effect and daily health product |
| CN104351329A (en) * | 2014-11-13 | 2015-02-18 | 山东商业职业技术学院 | Composite leaching vegetable fresh-keeping agent for tragus berteronianus and preparation method of fresh-keeping agent |
| CN104351329B (en) * | 2014-11-13 | 2017-02-08 | 山东商业职业技术学院 | Composite leaching vegetable fresh-keeping agent for tragus berteronianus and preparation method of fresh-keeping agent |
| CN107823023A (en) * | 2017-12-21 | 2018-03-23 | 李冬梅 | A kind of natural plant extracts composition and its application in cosmetics |
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