CN112089750A - Scutellaria baicalensis extract powder, and extraction method and application thereof - Google Patents
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Abstract
The invention relates to scutellaria baicalensis extract powder, an extraction method and application thereof, wherein the extraction method comprises the steps of sequentially crushing scutellaria baicalensis medicinal materials, extracting with water, concentrating, diluting, adjusting acidity, standing and precipitating, washing, drying and crushing. The extraction method of the baicalin extract powder increases the steps of concentration and dilution on the basis of the existing water extraction and acid precipitation extraction method, improves the steps of acid precipitation and washing, promotes the precipitation of medicinal material active ingredients in the extracting solution to the greatest extent, reduces the loss in the extraction step, greatly improves the content of baicalin in the baicalin extract powder, and solves the problem of low quality of downstream preparations caused by low content of the baicalin serving as a traditional Chinese medicinal active ingredient in the baicalin extract powder in the prior art.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to scutellaria baicalensis extract powder, and an extraction method and application thereof.
Background
Radix scutellariae, also known as camellia root and native gold tea root, is a perennial herb of scutellaria of the family labiatae, is bitter in taste and cold in nature, and has the effects of clearing heat, drying dampness, purging fire, detoxifying, stopping bleeding, preventing miscarriage and the like by taking root as a medicine. It can be used for treating epidemic febrile disease, upper respiratory infection, cough due to lung heat, yellow gallbladder due to damp-heat, pneumonia, dysentery, hemoptysis, conjunctival congestion, threatened abortion, hypertension, carbuncle, furuncle, and sore. In the production of Chinese medicinal preparation, the extract of scutellaria root, such as scutellaria root extract powder, is usually used as medicine, and its main active component is baicalin, which is an important component in sanhuang tablet. The content of baicalin which is an effective ingredient of the scutellaria baicalensis extract prepared by a water extraction and acid precipitation method in the prior art is not high, the drug effect and the quality of a downstream preparation are influenced, and the problem to be solved is urgent.
Disclosure of Invention
The invention aims to provide scutellaria baicalensis extract powder, an extraction method and application thereof, wherein the extraction method optimizes the existing method for extracting the scutellaria baicalensis extract powder by water extraction and acid precipitation, so that the content of scutelloside in the scutellaria baicalensis extract powder obtained by final extraction is obviously improved, and the problems in the prior art are solved.
The invention adopts the following technical scheme:
a method for extracting radix Scutellariae extract powder comprises the following steps:
(1) weighing scutellaria baicalensis, crushing to obtain coarse scutellaria baicalensis powder, carrying out water extraction on the coarse scutellaria baicalensis powder, filtering after the water extraction is finished, and collecting filtrate to obtain water extract;
the Scutellariae radix coarse powder refers to powder which can completely pass through a first sieve with the mesh inner diameter of 2000 μm + -70 μm, but is mixed with no more than 20% of powder which can pass through a third sieve with the mesh inner diameter of 355 μm + -13 μm. Preferably, the water extraction is to add the scutellaria baicalensis coarse powder into 9-11 times of boiling water for carrying out first reflux decoction for 1-2 hours, and then filter and collect filtrate to obtain a first extracting solution; adding 7-9 times of water into the reaction residue after the first reflux decoction for carrying out second reflux decoction for 0.5-1.5h, filtering after the second reflux decoction is finished, and collecting filtrate to obtain a second extracting solution; adding 5-7 times of water by weight into the reaction residue subjected to the second reflux decoction, performing third reflux decoction for 30-50min, filtering, and collecting filtrate to obtain a third extract; and combining the first extracting solution, the second extracting solution and the third extracting solution to obtain the water extracting solution.
(2) Concentrating the water extract to obtain a concentrated solution; preferably, the concentration is carried out until the density is 1 g/mL-1.2 g/mL, and more preferably, the concentration is carried out until the density is 1.2 g/mL; the water extract after reflux decoction is concentrated to the range, so that the volume of the solution can be reduced, and the subsequent washing procedure is facilitated.
(3) Diluting the concentrated solution to obtain a diluted solution; preferably, the dilution is to add 2-4 times of water by mass into the concentrated solution and mix the solution evenly. The dilution concentrated solution makes the effective components of the Chinese medicinal materials easier to settle.
(4) Heating the diluent to 70-90 ℃, and then adding hydrochloric acid to adjust the pH value to 2.0; experiments show that the control of acidity is crucial, and the extraction rate of baicalin is reduced when the pH value is lower than or higher than 2.0, so that the pH value needs to be controlled and adjusted to 2.0.
(5) Keeping the diluted solution after the pH value is adjusted at the temperature of 70-90 ℃, standing for precipitation, filtering, and discarding the filtrate to obtain a precipitate; the temperature of the heat preservation and standing is preferably 80 ℃, the time of the heat preservation and standing is preferably 3-18h, and then the filtration is carried out while the solution is hot; experiments prove that when the temperature of the heat-preservation standing and the time of the heat-preservation standing are controlled within the range, higher baicalin extraction rate can be obtained, particularly, the influence of the heat-preservation standing time on the baicalin extraction rate is larger, the total content of baicalin is in a descending trend along with the time extension, and the content of baicalin is in a remarkable descending trend after the heat-preservation standing time is longer than 18 hours.
(6) Washing the precipitate with ethanol and water in sequence, drying, and pulverizing to obtain Scutellariae radix extract powder. Preferably, the water washing is carried out until the pH value is 5-7 by adopting the mass concentration of 20-40% of ethanol and the dosage of the ethanol is 1-5% of the mass of the baical skullcap root coarse powder. The traditional washing method needs to use a large amount of water to wash the acid solution, so that not only is the washing time long and a large amount of water resources are wasted, but also the extract is lost along with water in the washing process, so that the content of the active ingredient baicalin is reduced, and the drug effect is influenced. Tests prove that compared with the traditional washing method, the method of firstly washing by using the ethanol with the specific mass concentration and then washing by using water has great influence on the content of the baicalin in the prepared scutellaria baicalensis extract powder, the content of the baicalin is increased from 72.52% to 83.93%, and the washing method is more efficient than the traditional washing method and saves water resources.
The scutellaria baicalensis extract powder extracted by the extraction method contains high-content baicalin, so that the scutellaria baicalensis extract powder can be used for preparing a medicinal preparation taking the scutellaria baicalensis extract as a raw material medicine. For example, the three-yellow tablet is used for preparing the three-yellow tablet, is derived from a classic famous prescription 'three-yellow heart-fire-purging decoction' in golden-deficient herbal medicine written in Zhongjing of medical holy Zhang, consists of rhubarb, scutellaria baicalensis extractum and berberine hydrochloride, has a dosage ratio of 300:21:5, is collected in Chinese pharmacopoeia of the calendar edition, and has the effects of clearing heat and removing toxicity, purging pathogenic fire and relaxing bowels. Can be used for treating conjunctival congestion, swelling, carbuncle, aphtha, sore throat, gingival swelling and pain, vexation, thirst, yellow urine, and constipation due to excessive heat in triple warmer; it is also used for acute enteritis and dysentery.
The invention has the beneficial effects that:
the extraction method of the scutellaria baicalensis extract powder increases the procedures of concentration and dilution of the concentrated solution on the basis of the existing water extraction and acid precipitation extraction method, and concentrates the solution after reflux decoction, so that the volume of the solution can be reduced, the subsequent washing procedure is facilitated, and the effective components in the medicinal materials are easier to precipitate by diluting the concentrated solution. The invention also improves the procedures of acid precipitation and washing, promotes the precipitation of the medicinal material active ingredients in the extracting solution to the greatest extent, reduces the loss in the procedures, greatly improves the content of baicalin in the baicalin extract powder by the extraction method, and solves the problem of low quality of downstream preparations caused by low content of the medicinal active ingredients baicalin the baicalin extract powder in the prior art.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
The embodiment provides an extraction method of scutellaria baicalensis extract powder, which comprises the following steps:
(1) weighing radix scutellariae, and crushing to obtain coarse radix scutellariae powder; firstly, adding coarse scutellaria baicalensis powder into boiling water with the weight being 9 times that of the coarse scutellaria baicalensis powder, carrying out first reflux decoction for 1 hour, filtering after the first reflux decoction is finished, and collecting filtrate to obtain a first extracting solution; adding 7 times of water by weight into the reaction residues subjected to the first reflux decoction for carrying out second reflux decoction for 0.5h, filtering after the second reflux decoction is finished, and collecting filtrate to obtain a second extracting solution; adding 5 times of water by weight into the reaction residue subjected to the second reflux decoction for carrying out third reflux decoction for 30min, and filtering and collecting filtrate after the third reflux decoction is finished to obtain a third extract; combining the first extract, the second extract and the third extract to obtain the water extract;
(2) concentrating the water extract until the density is 1g/mL to obtain a concentrated solution;
(3) adding 2 times of water by mass into the concentrated solution, and uniformly mixing to obtain a diluted solution;
(4) firstly, heating the diluent to 70 ℃, and then slowly adding 1mol/L hydrochloric acid while stirring to adjust the pH value to 2.0;
(5) keeping the diluted solution after the pH value is adjusted at 70 ℃ and standing for 18h to precipitate, filtering while the solution is hot, and then discarding the filtrate to obtain a precipitate;
(6) washing the precipitate with ethanol (mass concentration of 40%) 1% of the weight of the Scutellariae radix coarse powder, washing the precipitate with water until pH is 5, drying, and pulverizing to obtain Scutellariae radix extract powder.
Example 2
The embodiment provides an extraction method of scutellaria baicalensis extract powder, which comprises the following steps:
(1) weighing radix scutellariae, and crushing to obtain coarse radix scutellariae powder; firstly, adding coarse scutellaria baicalensis powder into boiling water with the weight being 11 times that of the coarse scutellaria baicalensis powder, carrying out first reflux decoction for 2 hours, filtering after the first reflux decoction is finished, and collecting filtrate to obtain a first extracting solution; adding 9 times of water by weight into the reaction residues subjected to the first reflux decoction for carrying out second reflux decoction for 1.5h, filtering after the second reflux decoction is finished, and collecting filtrate to obtain a second extracting solution; adding 7 times of water by weight into the reaction residue subjected to the second reflux decoction for carrying out third reflux decoction for 50min, and filtering and collecting filtrate after the third reflux decoction is finished to obtain a third extract; combining the first extract, the second extract and the third extract to obtain the water extract;
(2) concentrating the water extract until the density is 1.2g/mL to obtain a concentrated solution;
(3) adding 4 times of water by mass into the concentrated solution, and uniformly mixing to obtain a diluted solution;
(4) firstly, heating the diluent to 90 ℃, and then slowly adding 1mol/L hydrochloric acid while stirring to adjust the pH value to 2.0;
(5) keeping the diluted solution after the pH value is adjusted at 90 ℃ and standing for 3h to precipitate, filtering while the solution is hot, and then discarding the filtrate to obtain a precipitate;
(6) washing the precipitate with 5% ethanol (mass concentration of 20%) of Scutellariae radix coarse powder, washing the precipitate with water to pH 7, drying, and pulverizing to obtain Scutellariae radix extract powder.
Example 3
The embodiment provides an extraction method of scutellaria baicalensis extract powder, which comprises the following steps:
(1) weighing radix scutellariae, and crushing to obtain coarse radix scutellariae powder; firstly, adding the coarse powder of the scutellaria baicalensis into boiling water with the weight being 10 times that of the coarse powder of the scutellaria baicalensis, carrying out first reflux decoction for 1.5 hours, filtering after the first reflux decoction is finished, and collecting filtrate to obtain a first extracting solution; adding 8 times of water by weight into the reaction residues subjected to the first reflux decoction for carrying out second reflux decoction for 1 hour, and filtering and collecting filtrate after the second reflux decoction is finished to obtain a second extracting solution; adding 6 times of water by weight into the reaction residue subjected to the second reflux decoction for carrying out third reflux decoction for 40min, and filtering and collecting filtrate after the third reflux decoction is finished to obtain a third extract; combining the first extract, the second extract and the third extract to obtain the water extract;
(2) concentrating the water extract until the density is 1.2g/mL to obtain a concentrated solution;
(3) adding 3 times of water by mass into the concentrated solution, and uniformly mixing to obtain a diluted solution;
(4) firstly, heating the diluent to 80 ℃, and then slowly adding 1mol/L hydrochloric acid while stirring to adjust the pH value to 2.0;
(5) keeping the diluted solution after the pH value is adjusted at 80 ℃ and standing for 6 hours to precipitate, filtering while the solution is hot, and then removing the filtrate to obtain a precipitate;
(6) washing the precipitate with 2% ethanol (mass concentration of 40%) of Scutellariae radix coarse powder, washing the precipitate with water to pH 7, drying, and pulverizing to obtain Scutellariae radix extract powder.
Examples 4 to 12 and comparative examples 1 to 4 were carried out with one parameter being varied on the basis of example 3, see table 1 in particular.
TABLE 1
The baicalin content in the baicalin extract powder obtained by extraction in examples 3-12 and comparative examples 1-4 was measured, and the influence of pH, standing temperature and standing time on the baicalin extraction rate was examined, and the results are shown in Table 2.
TABLE 2 influence of pH on baicalin extraction yield
As can be seen from the above results, when the incubation time and temperature are constant, the pH of the solution is changed, and the baicalin content is obviously changed. Generally speaking, the baicalin content obtained by pH 2 is obviously improved compared with the baicalin content obtained by pH 1.0, 1.5 and 2.5, and experiments also find that the obtained baicalin extract with pH 1.0 has more amount than the baicalin extract with pH 2, but the content is reduced, which indicates that the baicalin extract with pH 1.0 contains more impurities compared with the latter, and the probable reason is that the strength of acid dropping can influence the precipitation rate of the baicalin, when the acidity is enhanced, the precipitation rate of the baicalin is increased, and inevitable impurities are carried and separated out, so that the quality of the baicalin extract is increased, and the baicalin extract is slowly dropped in the acid dropping process and is fully stirred.
TABLE 3 influence of incubation temperature on baicalin extraction yield
From the above results, it can be seen that when the acidity and the holding time are fixed, and the holding and standing temperature is changed, the baicalin extraction rate is the highest at the holding and standing temperature of 80 ℃, while the baicalin content is slightly reduced at the holding temperatures of 70 ℃ and 90 ℃, but the influence is not great.
TABLE 4 influence of incubation and standing time on baicalin extraction yield
As can be seen from the table above, when the acidity and the heat preservation temperature are constant, the influence of the heat preservation time of 3h, 6h, 9h, 12h, 18h and 24h on the baicalin extraction rate is respectively considered, and experiments show that when the heat preservation time is prolonged to 24h, the total content of the baicalin is in a descending trend, so the heat preservation standing time is preferably 3-18 h.
TABLE 5 Effect of washing pattern on baicalin extraction yield
The experimental result shows that the difference of the baicalin extraction rates is obvious by changing the washing mode, and more baicalin can be extracted by the washing mode of firstly washing with low-concentration ethanol and then washing with water. Therefore, the washing mode is preferably to wash with ethanol with the mass concentration of 20-40% and then wash with water until the pH value is 5-7.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The extraction method of the scutellaria baicalensis extract powder is characterized by comprising the following steps of:
(1) weighing radix scutellariae, and crushing to obtain coarse radix scutellariae powder; carrying out water extraction on the scutellaria baicalensis coarse powder, and filtering and collecting filtrate after the water extraction is finished to obtain water extract;
(2) concentrating the water extract to obtain a concentrated solution;
(3) diluting the concentrated solution to obtain a diluted solution;
(4) heating the diluent to 70-90 ℃, and then adding hydrochloric acid to adjust the pH value to 2.0;
(5) keeping the diluted solution after the pH value is adjusted at the temperature of 70-90 ℃, standing for precipitation, filtering, and discarding the filtrate to obtain a precipitate;
(6) washing the precipitate with ethanol and water in sequence, drying, and pulverizing to obtain Scutellariae radix extract powder.
2. The method for extracting scutellaria baicalensis extract powder according to claim 1, wherein in the step (1), the water extraction is to add scutellaria baicalensis coarse powder into boiling water with the weight of 9-11 times of that of the scutellaria baicalensis coarse powder for the first reflux decoction for 1-2 hours, and then filter and collect filtrate to obtain a first extracting solution; adding 7-9 times of water into the reaction residue after the first reflux decoction for carrying out second reflux decoction for 0.5-1.5h, filtering after the second reflux decoction is finished, and collecting filtrate to obtain a second extracting solution; adding 5-7 times of water by weight into the reaction residue subjected to the second reflux decoction, performing third reflux decoction for 30-50min, filtering, and collecting filtrate to obtain a third extract; and combining the first extracting solution, the second extracting solution and the third extracting solution to obtain the water extracting solution.
3. The method for extracting scutellaria baicalensis extract powder according to claim 1, wherein in the step (2), the concentration is carried out until the density is 1 g/mL-1.2 g/mL.
4. The method for extracting scutellaria baicalensis extract powder according to claim 1, wherein in the step (2), the concentration is carried out until the density is 1.2 g/mL.
5. The method for extracting scutellaria baicalensis extract powder according to claim 1, wherein in the step (3), the dilution is to add 2-4 times of water by mass into the concentrated solution and mix the mixture uniformly.
6. The method for extracting scutellaria baicalensis extract powder according to claim 1, wherein in the step (5), the temperature for keeping warm and standing is 80 ℃.
7. The method for extracting scutellaria baicalensis extract powder according to claim 1, wherein in the step (5), the heat preservation and standing are carried out for 3-18h, and then the filtration is carried out while the solution is hot.
8. The method for extracting scutellaria baicalensis extractum powder according to claim 1, wherein in the step (6), the mass concentration of the ethanol is 20-40%, the dosage of the ethanol is 1-5% of the mass of the scutellaria baicalensis coarse powder, and the water washing is carried out until the pH value is 5-7.
9. The extract powder of Scutellariae radix prepared by the extraction method of any one of claims 1-8.
10. The use of the scutellaria baicalensis extract powder of claim 9 in the preparation of a medicament with a scutellaria baicalensis extract as a bulk drug.
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