CN109045087B - Enrichment and purification process of rhus chinensis effective part - Google Patents
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Abstract
The invention discloses an enrichment and purification process of rhus chinensis effective parts, belongs to the field of purification of traditional Chinese medicine effective parts, and relates to a preparation method of rhus chinensis total phenolic acid parts, which comprises the following steps: (1) extraction: taking rhus chinensis powder, adding 50-70% ethanol for extraction, filtering, taking filtrate, and concentrating the filtrate under reduced pressure until no alcohol smell exists to obtain a rhus chinensis total phenolic acid solution; (2) and (3) macroporous resin purification: and (3) taking the rhus chinensis total phenolic acid solution, adsorbing by adopting macroporous resin, washing with water to remove impurities, and eluting by adopting 50-90% ethanol solution to obtain the rhus chinensis total phenolic acid. The method can obtain the rhus chinensis total phenolic acid yield, and provides a reasonable, economic and simple purification production process for the industrial production of the rhus chinensis total phenolic acid.
Description
Technical Field
The invention belongs to the field of purification of effective parts of traditional Chinese medicines, and particularly relates to an enrichment and purification process of effective parts of Rhus chinensis phenolic acids.
Background
Rhus chinensis Mill is a small arbor of deciduous genus of Rhus genus of Anacardiaceae family. According to records in Kaibao materia Medica, rhus chinensis has the effects of dispelling wind and eliminating dampness, reducing swelling and softening hard masses, promoting the production of body fluid and moistening lung, reducing pathogenic fire and reducing phlegm, astringing and detoxifying and the like, and is commonly used for treating symptoms such as lung deficiency cough, chest pain and the like. The traditional Chinese medicine considers that the rhus chinensis has the effects of inducing diuresis to alleviate edema, promoting blood circulation to remove blood stasis, dissipating qi and relieving pain. According to modern pharmacological studies, rhus chinensis has the effect of improving coronary circulation and hemorheology.
The research shows that the total phenolic acid in the rhus chinensis has the effect of relieving heart failure and the like, and the research for optimizing the purification process of the effective part of the rhus chinensis by taking the total phenolic acid as an index does not exist at present. Such as Lijialin, Wu Su Zhen, Bishu Zhanyu, Rhus chinensis Total flavone extraction technology research [ J ]. Shizhen Chinese medicine, 2009,20(05): 1116-.
It is desirable to provide a process for preparing rhus chinensis total phenolic acid.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of rhus chinensis total phenolic acid parts.
The preparation method of the rhus chinensis total phenolic acid part comprises the following steps:
(1) extraction: taking rhus chinensis powder, adding 50-70% ethanol for extraction, filtering, taking filtrate, and concentrating the filtrate under reduced pressure until no alcohol smell exists to obtain a rhus chinensis total phenolic acid solution;
(2) and (3) macroporous resin purification: taking a rhus chinensis total phenolic acid solution, dynamically adsorbing by adopting macroporous resin, washing with water to remove impurities, and eluting by adopting a 50-90% ethanol solution to obtain the rhus chinensis total phenolic acid.
In the step (1), the dynamic adsorption means that the rhus chinensis total phenolic acid solution passes through macroporous resin at a certain speed, and the target component is adsorbed on the resin.
In the step (1), the rhus chinensis powder is powder sieved by a 45-mesh sieve.
In the step (1), the material-to-liquid ratio of the rhus chinensis rhizome powder to the ethanol is 1 (20-25), preferably 1: 20.
in the step (1), the extraction is reflux extraction; and/or the extraction time is 60-90 min.
In the step (1), the number of extraction times is 2.
In the step (2), the model of the macroporous resin is HPD-600, HP2MGL, SP825L, preferably SP 825L.
In the step (2), the diameter-height ratio of the macroporous resin column is 1:5, 1:10, 1:15, preferably 1: 5.
In the step (2), the amount of the rhus chinensis total phenolic acid solution is that the mass ratio of the rhus chinensis total phenolic acid solution to the dry powder of the resin is 0.8: 1; and/or the dynamic adsorption speed is 1 BV.h-1。
In the step (2), the flow rate of the washing impurity removal is 1-3 BV.h-1Preferably 2 BV.h-1(ii) a And/or the amount of water is 4 BV.
In the step (2), the flow rate of the ethanol is 2-6 BV.h-1Preferably 2 BV.h-1。
According to the enrichment and purification process of the rhus chinensis effective part, the obtained extract has higher rhus chinensis total phenolic acid yield, and a reasonable, economic and simple purification production process is provided for industrial production of rhus chinensis total phenolic acid.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 Gallic acid Standard Curve
FIG. 2 solvent concentration as an influencing factor of total phenolic acid extraction
FIG. 3 shows the feed-to-liquid ratio of the influence factors on the total phenolic acid extraction yield
FIG. 4 extraction time of the influence of the total phenolic acid extraction yield
FIG. 5 extraction frequency of influence factors of total phenolic acid extraction
FIG. 612 comparison of static adsorption and desorption amounts of macroporous resins
FIG. 73 comparison of dynamic adsorption and desorption amounts of macroporous resins
FIG. 8SP825L resin leakage Curve examination result
FIG. 9 examination result of sample flow rate
FIG. 10 examination result of elution Curve
Detailed Description
Example 1 Total phenolic acid enrichment purification Process
(1) Extracting rhus chinensis total phenolic acid:
weighing 300g of coarse powder of rhus chinensis after being crushed and sieved (45 meshes), adding 20 times of 70% ethanol solution in volume fraction, soaking for 30min before extraction, then extracting for 90min under reflux for 2 times, combining the two filtrates, and concentrating under reduced pressure until no alcohol smell exists to obtain the rhus chinensis total phenolic acid solution.
(2) Separating and purifying rhus chinensis total phenolic acid:
a. macroporous resin pretreatment:
fully soaking 9g of SP825L macroporous resin by using 95% ethanol, and carrying out wet column packing after 24h, wherein the diameter-height ratio of the macroporous resin column after column packing is 1: 5. Eluting the column bed with 95% ethanol until the effluent is mixed with 5 times of distilled water and no white turbidity appears, washing with large amount of distilled water until the effluent has no alcohol smell, and standing.
b. Separating and purifying total phenolic acid:
and (b) taking the rhus chinensis total phenolic acid extracting solution prepared in the step (1), and passing the extract through the macroporous resin treated in the step (a). The amount of the rhus chinensis total phenolic acid is determined by the mass ratio of the rhus chinensis total phenolic acid solution to the dry powder of the resin being 0.8: 1 sample loading at 1 BV.h-1Performing dynamic adsorption at the speed of (2); after complete adsorption, removing impurity solvent water by 4BV and removing impurity solvent water by 2 BV.h-1Eluting, adding 50% ethanol as 4BV enrichment solvent at 2 BV.h-1And (4) eluting. Collecting the eluent.
The advantageous effects of the present invention are specifically described below by way of experimental examples.
Experimental example 1 extraction of Rhus chinensis Total phenolic acids
Instrument and reagent
1 apparatus
Shimadzu UV-1800 visible spectrophotometer (Shimadzu, Japan), CPA225D one-hundred thousand balance (product of Sidoisi scientific instruments Co., Ltd.), SHB-III circulating water multi-purpose vacuum pump (Zhengzhou Changchengchun Kogyo Co., Ltd.), LX-07A type multi-function pulverizer (Shanghai Jiang Xin science Co., Ltd.), and HH-Z type digital display constant temperature water bath (Changzhou Guohu electric appliances).
2 reagent
Rhus chinensis (dried rhizome of Rhus chinensis Mill. of Fujian Chinese medicinal university) was identified by high-grade laboratory of Van Shiming of pharmaceutical college of Fujian Chinese medicinal university, and the sample was stored in the biomedical research and development center of Fujian Chinese medicinal university; gallic acid control (chinese institute for food and drug testing); anhydrous sodium carbonate (AR), phosphomolybdotungstic Acid Reagent (AR), and ethanol (AR) were purchased from chemical reagents of national drug group, Inc.
3 extraction method
3.1 preparation of the solution
3.1.1 control solutions: accurately weighing 12.5mg of gallic acid as reference substance in a 25mL brown volumetric flask, adding water to fully dissolve, diluting to 25mL, shaking up, accurately weighing 5mL to 25mL volumetric flask of subsequent filtrate, adding water to constant volume, and shaking up to obtain the final product. (the concentration in this case was 0.05 mg/mL).
3.1.2 test article solution: pulverizing rhizome of Rhus chinensis Mill, sieving with 45 mesh sieve, adding 70% ethanol, reflux extracting at 80 deg.C for 90min, filtering, precisely measuring 10mL of the subsequent filtrate, placing in 100mL brown volumetric flask, diluting with ultrapure water to 100mL, and shaking.
3.1.3 establishment of standard curve absorbs 0.05mg/mL gallic acid standard solution 0.5, 1.0, 2.0, 3.0, 4.0, 5.0mL, respectively puts into 25mL brown volumetric flasks, respectively adds each phosphomolybdic tungstic acid test solution 1mL, respectively precisely adds water 11.5, 11.0, 10.0, 9.0, 8.0, 7.0mL, dilutes to scale with 29% sodium carbonate solution, shakes evenly, stands for 35min, uses corresponding reagent as blank, and measures absorbance at 760nm wavelength according to ultraviolet-visible spectrophotometry (appendix VA of the version 2015 of Chinese pharmacopoeia). The absorbance (Y) was plotted as the ordinate and the detection concentration (X) was plotted as the abscissa, and the results were shown in FIG. 1. Linear regression gave the regression equation Y of 89.874X +0.0223 and R of 0.999. The results show that gallic acid has good linear relationship in the range of 1.0-10.0 μ g/mL.
3.2 Fulin phenol method determination of phenolic acid content precisely absorbs sample solution 0.5mL, puts in 25mL brown measuring flask, according to "3.1.3" method determination absorbance, substitutes standard curve, calculates phenolic acid concentration, thus calculates the total phenol content.
3.2 Single factor investigation
3.2.1 Effect of ethanol concentration on Total phenolic acid extraction
Accurately weighing 5g of Rhus chinensis Mill powder respectively, placing in 5 conical flasks, adding 15 times of 40%, 50%, 60%, 70%, 80% ethanol respectively, soaking for 30min, reflux extracting for 60min, measuring the content of total phenolic acid in Rhus chinensis Mill according to method 3.1.3, and examining the influence of ethanol concentration on the extraction rate of total phenolic acid in Rhus chinensis Mill. As can be seen from fig. 2, the total phenolic acid extraction rate and the ethanol concentration are positively correlated between the ethanol concentration of 40% and 70%, but the total phenolic acid extraction rate does not change much when the ethanol concentration is between 60% and 70%, and the total phenolic acid extraction rate decreases inversely with the increase of the ethanol concentration after the ethanol concentration of 70%. Ethanol is saved for consideration. Therefore, the concentration of the extraction solvent selected by multi-factor design is 50-70%.
3.2.2 Effect of extract liquor ratio on Total phenolic acid extraction
Accurately weighing 5g of Rhus chinensis Mill powder respectively, placing in 5 conical flasks, adding 70% ethanol in an amount of 5, 10, 15, 20 and 25 times of the amount of the Rhus chinensis Mill powder respectively, soaking for 30min, reflux extracting for 60min, measuring the content of total phenolic acid in Rhus chinensis Mill according to the method of 3.1.3, and examining the influence of feed liquid ratio on the extraction rate of total phenolic acid in Rhus chinensis Mill. As shown in FIG. 3, the total phenolic acid extraction rate gradually increased with the increase of the feed-to-liquid ratio, and was substantially stable after the feed-to-liquid ratio was 1: 20. Therefore, the ratio of the materials to the liquid is 1: 15-1: 25.
3.2.3 Effect of extraction time on Total phenolic acid extraction
Accurately weighing 5g of Rhus chinensis Mill powder respectively, placing in a conical flask, adding 20 times of 70% ethanol, soaking for 30min, reflux extracting for 30min, 60min, 90min, 120min and 150min respectively, measuring the content of total phenolic acid in Rhus chinensis Mill according to method 3.1.3, and examining the influence of extraction time on the extraction rate of total phenolic acid in Rhus chinensis Mill. As a result, as shown in FIG. 4, the total phenolic acid extraction rate gradually increased with the increase of the extraction time, but the total phenolic acid extraction rate was substantially unchanged after the extraction time was 90 min. In order to reduce the extraction time. Therefore, the extraction time of the multi-factor design selection is 60-120 min.
3.2.4 Effect of extraction times on Total phenolic acid extraction
Accurately weighing 5g of rhus chinensis powder, placing the rhus chinensis powder in a conical flask, adding 20 times of 70% ethanol for soaking for 30min, performing reflux extraction for 90min, filtering to obtain a primary extracting solution, adding 20 times of 70% ethanol into filter residue, performing extraction with the primary extracting solution to obtain a secondary extracting solution, performing operation with the secondary extracting solution on the tertiary extracting solution, respectively measuring the content of total phenolic acid in the rhus chinensis in the primary extracting solution and the secondary extracting solution before and after according to the method 3.1.3, and inspecting the influence of the extraction times on the extraction rate of the total phenolic acid in the rhus chinensis. As a result, as shown in fig. 5, the extraction rate was the highest in the first time, and the extraction rate of total phenolic acids was almost 0 in the second time and the third time, and therefore the number of extraction times for the multifactorial examination was 2.
3.2.5 multifactor test
The multi-factor test method optimizes the extraction conditions of the total phenolic acid in the rhus chinensis, synthesizes the results of the single-factor test, takes the material-liquid ratio, the extraction time, the extraction times and the ethanol concentration as the investigation factors, and takes the extraction rate of the total phenolic acid as the response value to design the test, which is shown in table 1 and table 2.
TABLE 1 Multi-factor test Each factor level table
The multi-factor experimental schedule and results are shown in table 2:
TABLE 2 multifactor test arrangement and results
As shown in Table 2, when the extraction solvent is 50-70% ethanol, the ratio of material to liquid is 1 (20-25), the extraction frequency is 2, the extraction time is 60-90 min (test numbers are 2, 9 and 10), the extraction rate is high, preferably, the extraction solvent is 50-70% ethanol, the ratio of material to liquid is 1:20, the extraction frequency is 2, and the extraction time is 90min (test numbers are 2 and 10), the extraction rate exceeds 3.5%; the optimal reflux extraction process is A3B2C2D2Extracting with 70% ethanol at a ratio of 1:20 for 2 times for 90 min. According to the multi-factor experimental result, the optimal extraction mode is as follows: adding 70% ethanol 20 times the amount of 5g of Rhus chinensis Mill into the extract, soaking for 30min before extraction, reflux extracting for 90min,extracting for 2 times before and after.
Experimental example 2 purification of Rhus chinensis Total phenolic acids
Apparatus and materials
1 apparatus
UV9100 model ultraviolet visible spectrophotometer (beijing rayleigh analytical instruments corporation); one hundred thousand analytical balances of the CPA225D type (Sartorius, germany); one-ten-thousandth balance (sidoris scientific instruments ltd); KQ-500E ultrasonic cleaner (Kunshan ultrasonic Instrument Co., Ltd.); model FY135 Chinese herbal medicine grinder (Tester instruments, Inc. of Tianjin); HC-2068 high-speed centrifuge (Anhui Zhongjia scientific instruments, Inc.); model ZHWY-200D isothermal culture shaker (Shanghai Zhicheng Analyzer manufacturing Co., Ltd.); RE-2000A rotary evaporator (Shanghai Yangrong Biochemical Instrument factory); SHB-III circulating water type multipurpose vacuum pump (Zhengzhou great wall science and trade Co., Ltd.); KW-1000DC type constant temperature water bath HH-1 (national electric appliances Co., Ltd.); and (5) an oven.
2 reagent
Rhus chinensis extracting solution: dried rhizome of Rhuscarinensis Mill is identified by Rhuscarinensis (dried rhizome of Rhuscarinensis Mill.) of Mitsuga (batch No. 15122201, Anhui synergetic Reation decoction pieces Co., Ltd.) and high-grade laboratory of Hoffia chinensis university, and is extracted with 20 times of 70% ethanol under reflux for 90min, and the total phenolic acid is obtained by extracting 2 times to obtain 4.73 mg/mL-1The extract of (4).
A gallic acid control (China institute for food and drug assay, batch No. 110831-201204); macroporous resins HPD-100, HPD-300, HPD-450, HPD-600, HPD-700, AB-8, DM-130, D101, XAD-2 (Canon sorbent materials science, Inc.), macroporous resins HP-20, HP2MGL, SP825L (Green hundred grass science, Inc.); anhydrous sodium carbonate (AR), phosphomolybdotungstic Acid Reagent (AR), and ethanol (AR) were purchased from chemical reagents of national drug group, Inc.
3 purification method
3.1 macroporous resin screening
3.1.1 macroporous resin pretreatment
Fully soaking the macroporous resin with 95% ethanol, performing wet column packing after 24h, eluting a column bed with 95% ethanol until effluent liquid is mixed with 5 times of distilled water and no white turbidity appears, washing with a large amount of distilled water until the effluent liquid has no alcohol smell, and standing for later use.
3.1.2 static adsorption-desorption experiments
Weighing 2g of 12 processed macroporous resins (HPD-100, HPD-300, HPD-450, HPD-600, HPD-700, AB-8, DM-130, HP-20, HP2MGL, SP825L, D101 and XAD-2), respectively adding 10mL of Rhus chinensis extract, placing in a 50mL centrifuge tube, and placing in a constant temperature shaking table at a rotation speed of 150r min-1Oscillating for 24h at 37 ℃, taking out and centrifuging respectively, measuring the volume of the adsorption residual liquid, measuring the value A, and calculating the concentration of the adsorption liquid. And (3) after the 12 kinds of macroporous resins subjected to static adsorption are sucked dry by a liquid transfer gun, respectively adding 20mL of 95% ethanol into a 50mL centrifuge tube, measuring the volume of the desorption solution, measuring the value A of the desorption solution, and calculating the total phenolic acid concentration of the desorption solution. The static adsorption amount, desorption amount, adsorption rate and resolution rate were calculated according to the formulas 1-1 and 1-2.
Adsorption capacity ═ C0-C1)V1M, desorption amount ═ C2×V2/m (1-1)
Adsorption rate ═ C0-C1)/C0The resolution is (C)2×V2)/((C0-C1)×V)) (1-2)
Wherein: c0Concentration of total phenolic acid in the sample solution before adsorption (mg. mL)-1)，C1Concentration of total phenolic acids in the raffinate (mg. mL)-1)，C2Concentration of total phenolic acid in stripping solution (mg. mL)-1)，V1Volume of raffinate adsorbed (mL), V2Volume of stripping solution (mL), m-mass of dry resin (g).
The results are shown in Table 3 and FIG. 6. It is known that the adsorption rates of HPD-600, HP2MGL and SP825L on rhus chinensis total phenolic acid are all over 58% and the resolution rates are all over 45%. The adsorption and desorption effects of the three resins are not very different, so the three resins are selected for further dynamic adsorption investigation, and the optimal resin is selected.
TABLE 312 comparison of static adsorption and desorption of macroporous resins
3.1.3 dynamic adsorption experiments
Transferring 3 parts of Rhus chinensis Mill extract, each 30mL, respectively passing through 3 types (HPD-600, HP2MGL, SP825L) of treated macroporous resin columns (dry resin amount 9g), and performing dynamic adsorption; after complete adsorption, the column was washed with sufficient water until the effluent was nearly colorless, and then eluted with 90mL of 95% ethanol. Collecting the residual solution and ethanol eluate in turn, measuring the amount of total phenolic acid in each solution, and screening the best resin by using the adsorption amount, adsorption rate, analysis amount and analysis rate as evaluation indexes. As shown in table 4 and fig. 7, the SP825L macroporous resin showed relatively good adsorption, desorption and resolution of total phenolic acids in rhus chinensis, so SP825L resin was finally selected as the purification resin for rhus chinensis extract.
Table 43 macroporous resin dynamic adsorption investigation
3.2 Process for separating and purifying total phenolic acid by SP825L resin
3.2.1 examination of the amount of total phenolic acids in Rhus chinensis
The concentration of the sample was measured to be 0.3 g/mL-1The total phenolic acid of rhus chinensis is 30mL, and the total phenolic acid is 0.45 BV.h-1Dynamic adsorption was performed by passing the treated SP825L type macroporous resin column (9 g dry resin) at a flow rate of (1BV ═ 20 ml); effluent liquid is collected in sections, one part of effluent liquid is collected every 3mL, the content of the total phenolic acid is measured, and a corresponding leakage curve is drawn. The results are shown in FIG. 8, from which it can be seen that the initial effluent A value is particularly low and the adsorption efficiency is good, and that when the loading is increased to 24mL, significant leakage begins and the saturation adsorption is gradually approached. In order to reduce the loss of effective components, the maximum sample amount of the total phenolic acid of rhus chinensis is determined to be 24mL, and the sample amount is 0.8g converted into the total phenolic acid of rhus chinensis-1(Rhus chinensis total phenolic acids/resins).
3.2.2 investigation of sample flow Rate of Total phenolic acids from Rhus chinensis
Weighing three parts of Rhus chinensis extract, and sampling with 25mL of sample solution at a rate of 1 BV.h-1、2BV·h-1、3BV·h-1Adsorbing with treated SP825L macroporous resin column (dry resin content 9g) at flow rate of 1BV ═ 20mL, taking out the adsorption residual liquid, measuring the volume of residual liquid, eluting with 30mL 95% ethanol, desorbing, measuring the volume of desorption liquid, and measuring the total phenolic acid content of adsorption residual liquid and desorption liquid. As shown in Table 5 and FIG. 9, the adsorption rate decreased with the increase of the adsorption flow rate, and when the flow rate was small, the sample liquid was in contact with the resin for a relatively long time and was sufficiently adsorbed by the resin, thereby increasing the adsorption rate, and finally the optimum adsorption flow rate was determined to be 1 BV. h-1。
TABLE 5 investigation results of sample flow rates
3.3.3 examination of elution Curve
Weighing 120mL of rhus chinensis extract, and performing dynamic adsorption through a treated SP825L macroporous resin column (the dry resin amount is 54 g); after complete adsorption, the mixture is respectively treated with water and ethanol with different concentrations (30%, 50% and 95%) at a temperature of 2 BV.h-1Elution was performed at the flow rate. The eluate was collected at each 1BV (80 mL for 1 BV), the dry extract weight and content of each fraction were measured, and an elution curve was plotted with the number of erlenmeyer flasks as abscissa and the content as ordinate. As shown in table 6 and fig. 10, it is understood that almost no total phenolic acid was eluted with water, a small amount of total phenolic acid began to be eluted with 30% ethanol, and total phenolic acid adsorbed in the resin was almost completely eluted with 50% ethanol. Therefore, the optimal purification experimental method comprises the following steps: water is used as an impurity removal solvent, 50% ethanol is used as an enrichment solvent, and the using amount of the water is 4 BV.
TABLE 6 measurement results of total phenolic acid content of elution curve
3.3.4 selection of flow Rate and aspect ratio by multifactor method
Measuring 9 parts of rhus chinensis extract, wherein the sample solution is 20mL each, passing through treated SP825L macroporous resin columns (dry resin amount is 9g) with different diameter-height ratios, and examining the flow rate of a main factor impurity removal solvent, the flow rate of an enrichment solvent and the diameter-height ratio in the separation and purification process by adopting multiple factors (see table 7) to determine the better resin purification process conditions.
TABLE 7 multifactor design factor horizon
TABLE 8 multifactor design test results
As can be seen from Table 8, the most preferred combination is a diameter to height ratio of 1:5 and an impurity removal flow rate of 2 BV.h-1The enrichment flow rate is 2 BV.h-1。
The best separation method obtained by the experiment is as follows: selecting SP825L macroporous resin, wherein the content of rhus chinensis total phenolic acid is as follows: rhus chinensis Total phenolic acid 0.8g-1Dry resin, adsorption flow rate: 1 BV. h-1The impurity removal solvent is water, the using amount is 4BV, the solvent for enriching the total phenolic acid is 50 percent ethanol, the using amount is 4BV, and the diameter-height ratio is as follows: 1:5, impurity removal flow rate: 2 BV. h-1And the enrichment flow rate: 2 BV. h-1。
The method can improve the yield of the rhus chinensis total phenolic acid, and provides a reasonable, economic and simple purification production process for the industrial production of the rhus chinensis total phenolic acid.
Claims (8)
1. A preparation method of rhus chinensis total phenolic acid parts is characterized by comprising the following steps: it comprises the following steps:
(1) extraction: taking rhus chinensis rhizome powder, adding 50-70% ethanol for extraction, filtering, taking filtrate, and concentrating the filtrate under reduced pressure until no alcohol smell exists to obtain a rhus chinensis total phenolic acid solution; the material-liquid ratio of the rhus chinensis rhizome powder to the ethanol is 1 (20-25); the extraction is reflux extraction; the extraction time is 60-90 min;
(2) and (3) macroporous resin purification: taking a rhus chinensis total phenolic acid solution, dynamically adsorbing by adopting macroporous resin, washing with water to remove impurities, and eluting by adopting a 50-90% ethanol solution to obtain rhus chinensis total phenolic acid; the model of the macroporous resin is HPD-600, HP2MGL and SP 825L; the diameter-height ratio of the macroporous resin column is 1:5, 1:10 and 1: 15; the amount of the rhus chinensis total phenolic acid solution is that the mass ratio of the rhus chinensis total phenolic acid solution to the dry powder of the resin is 0.8: 1; the dynamic adsorption speed is 1 BV.h-1(ii) a The flow rate of the washing impurity removal is 1-3 BV.h-1(ii) a The using amount of water is 4 BV; the flow rate of the ethanol solution is 2-6 BV.h-1。
2. The method of claim 1, wherein: in the step (1), the rhus chinensis rhizome powder is powder which is sieved by a 45-mesh sieve.
3. The method of claim 1, wherein: in the step (1), the material-to-liquid ratio of rhus chinensis rhizome powder to ethanol is 1: 20.
4. the method of claim 1, wherein: in the step (1), the number of extraction times is 2.
5. The method of claim 1, wherein: in the step (2), the model of the macroporous resin is SP 825L.
6. The method of claim 1, wherein: in the step (2), the diameter-height ratio of the macroporous resin column is 1: 5.
7. According to claimThe method of claim 1, wherein: in the step (2), the flow rate of the washing impurity removal is 2 BV.h-1。
8. The method of claim 1, wherein: in the step (2), the flow rate of the ethanol solution is 2 BV.h-1。
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| CN116077540B (en) * | 2021-11-08 | 2024-01-12 | 中国医学科学院药物研究所 | Application of Rhus chinensis extract in preparing medicine for treating stomach-related diseases |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101085010A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力制药股份有限公司 | Composition containing rhus chinensis for treating cardiovascular diseases and its preparation |
| WO2009133351A3 (en) * | 2008-04-28 | 2010-06-17 | Naturally Scientific Energy Limited | Production of biofuel from plant tissue culture sources |
| KR101735097B1 (en) * | 2016-04-05 | 2017-05-12 | 건국대학교 산학협력단 | Composition containing Rhus verniciflua extract for corrosion inhibition and the method of corrosion inhibition using the same |
| KR101772091B1 (en) * | 2016-05-26 | 2017-09-05 | 남명수 | Antibacterial fragrances composition and method for manufacturing antibacterial fragrances using the same |
| CN107362084A (en) * | 2017-07-28 | 2017-11-21 | 张家界久瑞健康产业发展有限公司 | A kind of facial mask containing Chinese sumac leaf extract and preparation method thereof |
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| CN106177020B (en) * | 2016-08-19 | 2017-11-17 | 中南民族大学 | The extraction of total phenolics and purifying process in a kind of wrinkled papaya |
| CN106551962B (en) * | 2016-11-21 | 2020-05-15 | 昆明理工大学 | Rhus chinensis fruit extract and preparation method and application thereof |
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| CN101085010A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力制药股份有限公司 | Composition containing rhus chinensis for treating cardiovascular diseases and its preparation |
| WO2009133351A3 (en) * | 2008-04-28 | 2010-06-17 | Naturally Scientific Energy Limited | Production of biofuel from plant tissue culture sources |
| KR101735097B1 (en) * | 2016-04-05 | 2017-05-12 | 건국대학교 산학협력단 | Composition containing Rhus verniciflua extract for corrosion inhibition and the method of corrosion inhibition using the same |
| KR101772091B1 (en) * | 2016-05-26 | 2017-09-05 | 남명수 | Antibacterial fragrances composition and method for manufacturing antibacterial fragrances using the same |
| CN107362084A (en) * | 2017-07-28 | 2017-11-21 | 张家界久瑞健康产业发展有限公司 | A kind of facial mask containing Chinese sumac leaf extract and preparation method thereof |
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