CN107349255B - Flocculation impurity removal process for scutellaria baicalensis extracting solution and application of flocculation impurity removal process - Google Patents
Flocculation impurity removal process for scutellaria baicalensis extracting solution and application of flocculation impurity removal process Download PDFInfo
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Abstract
The invention provides a flocculation impurity removal process for a scutellaria baicalensis extracting solution. The invention adopts the comprehensive application of the flocculating aid and the flocculating agent to destroy a colloid system in the water extract and remove impurities in advance, thereby reducing the hydrolysis of effective components and effectively improving the clarity of the extract, thereby effectively improving the content of the effective components of the scutellaria baicalensis extract and the yield of the baicalin. The method comprises the following specific steps: (1) adding coagulant aid suspension into the scutellaria baicalensis extracting solution, and uniformly stirring to obtain solution I; (2) heating the solution I, adding a flocculant solution into the solution I, and uniformly stirring the solution I to obtain a solution II; (3) adjusting the pH value of the solution II to 4.5-7.0, and then carrying out heat preservation and standing treatment; (4) and (4) taking the supernatant after standing in the step (3), filtering, and heating to adjust acid to obtain the baicalin precipitate.
Description
Technical Field
The invention belongs to the technical field of natural product extraction, and particularly relates to a flocculation impurity removal process for a scutellaria baicalensis extracting solution and application thereof.
Background
The Chinese medicinal material Scutellariae radix is dried root of Scutellaria baicalensis Georgi (Scutellaria baicalensis Georgi), has effects of clearing heat, removing toxic substance, stopping bleeding, preventing miscarriage, and also has strong antioxidation and anti-tumor effects, and its main effective component is baicalin.
At present, baicalin and baicalein in Chinese medicinal preparations and cosmetics are extracted from scutellaria baicalensis, and the content of the baicalin is used as a main technical index. The Scutellariae radix can be extracted by water extraction and acid precipitation, ultrasonic method, ultrafiltration, alcohol extraction and acid precipitation, microwave extraction, etc. The common method for industrial production is water extraction and acid precipitation (such as CN1454899, Hangui ru, etc.), which is used as the primary extraction process of Scutellariae radix, and has the advantages of simple process, low cost, high extraction rate, etc. However, as water is a low-price and high-efficiency solvent, in the process of dissolving out the effective component baicalin, a plurality of hydrophilic impurities, such as macromolecular substances, such as starch, protein, polyhydroxy tannin and the like, are also brought into a solution system to form a stable colloid-like solution. During acidification, the colloidal substances and baicalin form coprecipitation, so that the baicalin crystal form is thinned, the subsequent separation and purification are difficult, the product purity is low, and the product appearance is dark.
To solve the above problems, the general solutions are: (1) adding multi-step alkali-dissolution and acid-precipitation processes (such as CN104523833A, CN105497131A and the like), (2) adopting an alcohol-precipitation process (such as CN102266386A, CN103520277A and the like), (3) adding a flocculation clarifier (such as chitosan (Wanyan and the like; research on purification and impurity removal processes of a scutellaria baicalensis aqueous extract by chitosan [ J ]. Shizhen Chinese medical and national medicine, 2010,21(1):169 and 170; Chenzhang and the like; flocculation effect of chitosan on the scutellaria baicalensis decoction [ J ]. Chinese college of pharmacy, 1999(3):227 and 230), a commodity clarifier ZTC (Wufang and the like; research on flocculation processes of scutellaria baicalensis aqueous decoction [ J ]. Chinese herbal medicine, 2008,39(5):701 and 702), bentonite (CN1821257A) and the like by a uniform design method.
The flocculation settling method has the disadvantages of complex process, high cost, poor effect, difficulty in obtaining transparent supernatant, fluffy alum blossom, difficulty in filtering, and low extraction rate due to the fact that a large amount of useful solution is carried in the mud. Therefore, a new process for flocculating and removing impurities from the scutellaria baicalensis extracting solution is urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a flocculation impurity removal process for a scutellaria baicalensis extracting solution. The invention adopts the comprehensive application of the flocculating aid and the flocculating agent to destroy a colloid system in the water extract and remove impurities in advance, thereby reducing the hydrolysis of effective components and effectively improving the clarity of the extract, thereby effectively improving the content of the effective components of the scutellaria baicalensis extract and the yield of the baicalin.
Specifically, the technical scheme of the invention is as follows:
the invention discloses a flocculation impurity removal method of a scutellaria baicalensis extracting solution, which comprises the following steps:
(1) adding coagulant aid suspension into the scutellaria baicalensis extracting solution, and uniformly stirring to obtain solution I;
(2) heating the solution I, adding a flocculant solution into the solution I, and uniformly stirring the solution I to obtain a solution II;
(3) adjusting the pH value of the solution II to 4.5-7.0, and then carrying out heat preservation and standing treatment;
(4) and (4) taking the supernatant after standing in the step (3), filtering, and heating to adjust acid to obtain the baicalin precipitate.
Preferably, the preparation method of the scutellaria baicalensis extracting solution comprises the following steps: slicing Scutellariae radix, inactivating enzyme, extracting with water at 80-100 deg.C for 2-3 times, and mixing extractive solutions;
preferably, the coagulant aid is bentonite or sodium bentonite, and the concentration of the coagulant aid added into the solution I is 0-300 ppm; more preferably 100 to 300ppm; most preferably 200 ppm;
the coagulant aid suspension is prepared by adding a coagulant aid into water, and the mass fraction of the coagulant aid suspension is 1-10%;
preferably, the flocculant is one or more of calcium chloride, calcium nitrate, magnesium chloride and magnesium sulfate, further preferably, the flocculant is calcium chloride, calcium nitrate, magnesium chloride, magnesium sulfate, calcium chloride and calcium nitrate or magnesium chloride and magnesium sulfate, and it is required to be noted that the flocculant comprises a hydrate of a corresponding compound;
the addition amount of the flocculating agent is 0.1-1.0% of the mass of the scutellaria baicalensis extracting solution, and preferably 0.2-0.5%;
preferably, the heating temperature of the solution I in the step (2) is 80-90 ℃;
preferably, the heat preservation and standing treatment time is 1-2 h;
preferably, when the flocculating agent is calcium salt, the pH value of the solution II in the step (3) is 5.5-6.5;
when the flocculating agent is a magnesium salt, the pH value of the solution II in the step (3) is 5.0-6.0;
preferably, the heating temperature in the step (4) is 75-95 ℃, and hydrochloric acid is used for adjusting the pH of the solution to 1.5-2.
Preferably, the flocculation impurity removal method of the scutellaria baicalensis extracting solution further comprises the steps of filtering, washing and drying the baicalin precipitate prepared in the step (4) to obtain the baicalin extract.
The principle of the invention is as follows: the invention forms macromolecular colloid, polysaccharide substance, protein and tannin into co-suspension colloid by uniform dispersion and surface adsorption of negatively charged bentonite (sodium montmorillonite as main component) in colloid solution, and uses cationic flocculant Ca2+、Mg2+The addition of (2) promotes the colloid to flocculate to form alum floc. Through the synergistic action of the coagulant aid (flocculant aid) and the flocculant, a colloid system in the water extract is destroyed, and impurities are removed in advance, so that crystal entrainment during acid precipitation is reduced, and the aim of purifying products is fulfilled. The inventor finds in research that the dosage of the coagulant aid and the flocculantThe influence of the relation on flocculation impurity removal is huge, and the impurity removal effect is very poor if the addition range is separated from the preferable addition range of the invention; and other cationic flocculants (such as iron salt, aluminum salt and the like) can promote colloid flocculation to form alum floc precipitates, but the effect of impurity removal is poor, or a stable complex is formed with effective components of scutellaria baicalensis, so that the extraction rate is reduced.
In the second aspect of the invention, the application of the flocculation impurity removal method in the extraction process of high-purity scutellaria baicalensis extract and/or baicalin is disclosed. The method is particularly suitable for extracting the scutellaria baicalensis raw material with low content, and can effectively improve the extraction efficiency.
The invention has the beneficial effects that:
1) the flocculation impurity removal method can effectively accelerate the sedimentation of macromolecular impurities such as colloid, protein, starch and the like in the scutellaria baicalensis water extract, improve the clarity of the extract and facilitate subsequent filtration;
2) the coprecipitation of baicalin and impurities during acidification is reduced, and the purity of the final product is improved;
3) the sedimentation time is effectively reduced, and the hydrolysis of the effective components is reduced;
4) the process is shortened, the water consumption is reduced, and the yield is improved.
In a word, the invention has simple, reasonable and feasible process, safety and effectiveness, low cost, cheap raw materials, no need of large-scale expensive equipment and easy large-scale industrial production, thereby having great commercial popularization value.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular is intended to include the plural unless the context clearly dictates otherwise, and it should be further understood that when the term "comprises" or "comprising" is used in this specification, it indicates the presence of the feature, step, operation, device, component or group thereof.
As introduced in the background art, the flocculation impurity removal process aiming at the scutellaria baicalensis extracting solution still has various problems of complex process, high cost, unsatisfactory impurity removal effect and the like so far;
in view of the above, a typical embodiment of the present invention discloses a flocculation impurity removal method for a scutellaria baicalensis extracting solution, which comprises:
(1) adding coagulant aid suspension into the scutellaria baicalensis extracting solution, and uniformly stirring to obtain solution I;
(2) heating the solution I, adding a flocculant solution into the solution I, and uniformly stirring the solution I to obtain a solution II;
(3) adjusting the pH value of the solution II to 4.5-7.0, and then carrying out heat preservation and standing treatment;
(4) and (4) taking the supernatant after standing in the step (3), filtering, and heating to adjust acid to obtain the baicalin precipitate.
Wherein the preparation method of the scutellaria baicalensis extracting solution in the step (1) comprises the following steps: slicing Scutellariae radix, inactivating enzyme, extracting with water at 80-100 deg.C for 2-3 times, and mixing extractive solutions;
the coagulant aid is bentonite or sodium bentonite, and the concentration of the coagulant aid added into the solution I is 0-300 ppm; more preferably 100 to 300ppm; most preferably 200 ppm;
the coagulant aid suspension is prepared by adding a coagulant aid into water, and the mass fraction of the coagulant aid suspension is 1-10%;
the flocculant is one or more of calcium chloride, calcium nitrate, magnesium chloride and magnesium sulfate, and is further preferable to be calcium chloride, calcium nitrate, magnesium chloride, magnesium sulfate, calcium chloride and calcium nitrate or magnesium chloride and magnesium sulfate, and the flocculant comprises a hydrate of a corresponding compound;
the addition amount of the flocculating agent is 0.1-1.0% of the mass of the scutellaria baicalensis extracting solution, and preferably 0.2-0.5%;
the heating temperature of the solution I in the step (2) is 80-90 ℃;
the heat preservation standing treatment time is 1-2 h;
in another typical embodiment of the present invention, when the flocculant is calcium salt, the pH of the solution II in the step (3) is 5.5 to 6.5;
in another exemplary embodiment of the invention, when the flocculant is a magnesium salt, the pH of the solution II in the step (3) is 5.0-6.0;
in the step (4), the heating temperature is 75-95 ℃, and hydrochloric acid is used for adjusting the pH of the solution to 1.5-2.
In another exemplary embodiment of the present invention, the method for removing impurities by flocculation of the scutellaria baicalensis extracting solution further comprises filtering, washing and drying the baicalin precipitate prepared in step (4) to obtain the baicalin extract.
In another exemplary embodiment of the present invention, the application of the flocculation impurity removal method in the extraction process of high-purity scutellaria baicalensis extract and/or baicalin is disclosed. The flocculation impurity removal method is particularly suitable for extracting the scutellaria baicalensis raw material with low content, and can effectively increase the extraction efficiency.
The present invention will be further described with reference to the following examples and comparative examples, which are intended to be illustrative only and not limiting.
Example 1
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice, each for 1 hr, and mixing extractive solutions;
(2) keeping the temperature of the extracting solution at 80-90 ℃, adding 50g of the prepared bentonite (1%) suspension under stirring, uniformly stirring, and adjusting the pH value to 4.8 by using dilute hydrochloric acid;
(3) adding 42g of 20% calcium chloride solution prepared in advance at 80-90 ℃, and uniformly stirring;
(4) adjusting the pH value to 5.8-6.0 by 20% sodium hydroxide under stirring;
(5) keeping the temperature and standing, generating large flocculate precipitate, settling for 1-2 hours, sampling and checking the flocculation effect;
(6) filtering the supernatant;
(7) heating the filtrate to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(8) filtering, washing with water, and drying to obtain crude extract of baicalin.
Example 2
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice, each for 1 hr, and mixing extractive solutions;
(2) adding 42g of 20% calcium chloride solution prepared in advance at 80-90 ℃, and uniformly stirring;
(3) adjusting the pH value to 5.8-6.0 with 20% sodium hydroxide under stirring;
(4) keeping the temperature and standing, generating large flocculate precipitate, settling for 1-2 hours, sampling and checking the flocculation effect;
(5) filtering the supernatant;
(6) heating the filtrate to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(7) filtering, washing with water, and drying to obtain crude extract of baicalin.
Example 3
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice (1 hr each time), mixing extractive solutions, and weighing about 2500 g;
(2) keeping the temperature of the extracting solution at 80-90 ℃, adding 50g of the prepared bentonite (1%) suspension under stirring, uniformly stirring, and adjusting the pH value to 4.8 by using dilute hydrochloric acid;
(3) adding 42g of 20% magnesium chloride solution prepared in advance, and stirring for 10 min;
(4) adjusting pH to 5.2-5.5 with 20% sodium hydroxide;
(5) keeping the temperature and standing, generating large flocculate precipitate, settling for 1-2 hours, sampling and checking the flocculation effect;
(6) filtering the supernatant;
(7) heating the filtrate to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(8) filtering, washing with water, and drying to obtain crude extract of baicalin.
Example 4
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice (1 hr each time), mixing extractive solutions, and weighing about 2500 g;
(2) keeping the temperature of the extracting solution at 80-90 ℃, adding 50g of the prepared bentonite (1%) suspension under stirring, uniformly stirring, and adjusting the pH value to 4.8 by using dilute hydrochloric acid;
(3) 42g of 20% magnesium sulfate solution prepared in advance is added at 80-90 ℃, and the mixture is stirred for 10 min. At the moment, the pH value of the system is between 4 and 5;
(4) adjusting the pH value to 5.2-5.5 with 20% sodium hydroxide under stirring;
(5) keeping the temperature and standing, generating large flocculate precipitate, settling for 1-2 hours, sampling and checking the flocculation effect;
(6) filtering the supernatant;
(7) heating the filtrate to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(8) filtering, washing with water, and drying to obtain crude extract of baicalin.
Comparative example 1
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice (1 hr each time), mixing extractive solutions, and weighing about 2500 g;
(2) preserving the temperature of the extracting solution at 80-90 ℃, standing and settling for 1-2 hours, and sampling to check the flocculation effect;
(3) transferring the supernatant into an acidification tank;
(4) heating to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(5) settling, discharging supernatant, filtering lower layer precipitate, washing with water, and drying to obtain baicalin crude extract;
comparative example 2
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice, each for 1 hr, and mixing extractive solutions;
(2) keeping the temperature of the extracting solution at 80-90 ℃, adding 80g of chitosan solution (with the content of 1 percent and dissolved by 1 percent acetic acid solution) prepared in advance while stirring, and uniformly stirring;
(3) standing, keeping the temperature and settling for 1-2 hours, and sampling to check the flocculation effect;
(4) filtering the supernatant;
(5) heating the filtrate to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(6) filtering, washing with water, and drying to obtain crude extract of baicalin.
Comparative example 3
(1) Slicing Scutellariae radix 200g, heating with steam to inactivate enzyme, reflux-extracting with 1800ml water for 2 hr, reflux-extracting with 700ml × 2 water twice, each for 1 hr, and mixing extractive solutions;
(2) keeping the temperature of the extracting solution at 80-90 ℃, adding 40g of a pre-prepared commercial double-component flocculant solution (1 percent, prepared according to the use specification) while stirring, and uniformly stirring;
(3) at this time, the colloidal solution is destroyed, and large flocculate precipitation begins to be generated;
(4) stirring for 10min, sampling, checking the flocculation effect, standing, and carrying out heat preservation and sedimentation for 1-2 hours.
(5) Filtering the supernatant;
(6) heating the filtrate to 80-90 ℃, and adjusting the pH value to 1.5-2 by using hydrochloric acid to generate baicalin precipitate;
(7) filtering, washing with water, and drying to obtain crude extract of baicalin.
Comparative example 4
The method is the same as example 1 except that the pH in step (4) is adjusted to 4.8 to 5.0.
Comparative example 5
The method is the same as example 2 except that the pH in the step (4) is adjusted to 7.0 to 7.3.
Comparison of experimental results:
and (4) test conclusion:
the above examples and comparative examples show that the flocculation process of the present invention is applied to the production of scutellaria baicalensis extract, and has the characteristics of low cost, good flocculation effect, high clarity of supernatant, high settling speed, etc. The content of the effective components of the scutellaria baicalensis extract prepared by the process can be improved by about 5 percent, and the yield of the baicalin can be improved by more than 10 percent. Meanwhile, the fourth and fifth comparative examples show that the pH control requirement of the process is strict, the loss of effective components is caused when the pH is too high, the yield is obviously reduced, the turbidity of the supernatant is increased when the pH is too low, impurities are not thoroughly removed, and the content of the effective components of the product is low.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (9)
1. A flocculation impurity removal method of a radix scutellariae extracting solution is characterized by comprising the following steps:
(1) adding coagulant aid suspension into the scutellaria baicalensis extracting solution, and uniformly stirring to obtain solution I;
(2) heating the solution I, adding a flocculant solution into the solution I, and uniformly stirring the solution I to obtain a solution II;
(3) adjusting the pH value of the solution II and then carrying out heat preservation and standing treatment;
(4) taking the supernatant after standing in the step (3), filtering, and heating to adjust acid to obtain baicalin precipitate;
the coagulant aid is bentonite which is used as the coagulant aid,
the concentration of the coagulant aid added into the solution I is 100-300 ppm;
the flocculating agent is one or more of calcium chloride, calcium nitrate, magnesium chloride and magnesium sulfate, and the addition amount of the flocculating agent is 0.1-1.0% of the mass of the scutellaria baicalensis extracting solution;
when the flocculating agent is calcium salt, the pH value of the solution II in the step (3) is 5.5-6.5;
and (3) when the flocculating agent is a magnesium salt, the pH value of the solution II in the step (3) is 5.0-6.0.
2. The flocculation impurity removal method of scutellaria baicalensis extracting solution according to claim 1, wherein the preparation method of the scutellaria baicalensis extracting solution comprises the following steps: slicing Scutellariae radix, inactivating enzyme, extracting with water at 80-100 deg.C for 2-3 times, and mixing the extractive solutions.
3. A flocculation impurity removal method for scutellaria baicalensis extracting solution according to claim 1, wherein the concentration of the coagulant aid added in the solution I is 200 ppm.
4. The flocculation impurity removal method of scutellaria baicalensis extracting solution according to claim 1,
the addition amount of the flocculating agent is 0.2-0.5% of the mass of the scutellaria baicalensis extracting solution.
5. The flocculation impurity removal method for scutellaria baicalensis extracting solution according to claim 1, wherein the heating temperature of the solution I in the step (2) is 80-90 ℃.
6. The flocculation impurity removal method of scutellaria baicalensis extracting solution according to claim 1, wherein the heat-preservation standing treatment time is 1-2 h.
7. The flocculation impurity removal method for radix scutellariae extract according to claim 1, wherein the heating temperature in step (4) is 75-95 ℃, and hydrochloric acid is used to adjust the pH of the solution to 1.5-2.
8. The flocculation impurity removal method of scutellaria baicalensis extracting solution according to claim 1, further comprising filtering, washing and drying the baicalin precipitate prepared in the step (4) to obtain a baicalin extract.
9. Use of a flocculation decontamination method as claimed in any one of claims 1 to 8 in a process for extracting high purity scutellaria baicalensis extract and/or baicalin.
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