CN107375537B - Preparation method of tea polyphenol in southwest camellia - Google Patents
Preparation method of tea polyphenol in southwest camellia Download PDFInfo
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 78
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 78
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 240000001548 Camellia japonica Species 0.000 title claims description 57
- 241001122767 Theaceae Species 0.000 title abstract 3
- 239000011347 resin Substances 0.000 claims abstract description 51
- 229920005989 resin Polymers 0.000 claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000000605 extraction Methods 0.000 claims abstract description 41
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- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 10
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- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 244000269722 Thea sinensis Species 0.000 claims description 41
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- 238000002474 experimental method Methods 0.000 claims description 7
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/82—Theaceae (Tea family), e.g. camellia
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention provides a preparation method of tea polyphenol in camellia sinense, which comprises the steps of taking dried camellia sinense as a raw material, taking 50-80% acetone-water solution as a solvent for reflux extraction, concentrating and drying an extracting solution, dissolving the extracting solution in water, filtering, adsorbing a filtrate by DM130 macroporous resin, eluting impurities by distilled water, eluting by using 20-60% ethanol solution, collecting ethanol eluate, concentrating and drying to obtain a tea polyphenol product of the camellia sinense. The preparation method can effectively extract and enrich the total polyphenol in the southwest camellia, the produced total polyphenol has high purity and good quality, the composition and the structure of the polyphenol components can be effectively protected, the operation is simple, the cost is low, the used solvent can be recovered, the macroporous resin can be regenerated, and the preparation method is suitable for large-scale production.
Description
Technical Field
The invention relates to a preparation method of active components in natural medicine camellia southwest, in particular to a preparation method of tea polyphenol in camellia southwest.
Background
Southwest Camellia (Camellia pitardii), which is called southwest Camellia, is evergreen and evergreen shrub or small arbor of Camellia, and is produced in provinces such as Hunan, Guangxi, Yunnan, Guizhou and Sichuan of China. The camellia sinensis has the effects of promoting blood circulation, stopping bleeding, astringing to arrest diarrhea, detoxifying, healing sore and the like, and is mainly used for treating irregular menstruation, menorrhagia, intestinal wind, hematemesis, acute gastroenteritis, dysentery, rectocele, leucorrhea, spermatorrhea, rheumatic arthralgia, burn, scald and the like. The tea polyphenol in the southwest camellia flower is a representative polyphenol component obtained by enriching and purifying the southwest camellia flower. Modern pharmacological studies show that the camellia in southwest has pharmacological activities of resisting inflammation, resisting allergy and the like.
Therefore, the deep research on the process for extracting, purifying and enriching the tea polyphenol in the camellia sieboldii is necessary, the research on the process for enriching the tea polyphenol in the camellia sieboldii is less at present, most of the traditional process methods need to carry out treatments such as acid-base treatment, enzyme treatment, ultrasonic treatment and the like, the composition and the structure of total polyphenol can be influenced, the yield of the extract is low, impurities are more, great difficulty is brought to subsequent treatment, time and labor are wasted, and the development and the utilization of the medicinal value of the camellia sieboldii are not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the traditional technology and provides a preparation method for enriching and purifying tea polyphenol in high-purity southwest camellia.
In order to realize the purpose, the invention adopts the following technical scheme:
the preparation method of the tea polyphenol in the southwest camellia comprises the following steps:
(1) pulverizing dried raw materials of the southwest camellia;
(2) refluxing and extracting the camellia southwestern in the step (1) by taking 50-80% acetone-water solution as a solvent and taking the ratio (g: ml) of the camellia southwestern and the extraction solvent as 1: 10-40; extracting at the temperature of 60-100 ℃ for 1-5 h for 1-4 times, and combining the extracting solutions;
(3) screening out the extract with the highest total polyphenol yield through a single-factor experiment and an orthogonal experiment;
(4) concentrating and drying the extracting solution in the step (3), dissolving in water, and filtering;
(5) adsorbing the filtrate by using DM130 macroporous resin, eluting impurities by using distilled water with the resin amount (ml/g) being 3-5 times of that of the filtrate, eluting the impurities completely by using an ethanol solution with the concentration of 20-60% and the resin amount (ml/g) being 12-21 times of that of the filtrate, and collecting the eluent;
(6) screening the eluent with the highest total polyphenol content through a single-factor experiment;
(7) and (4) concentrating and drying the eluent obtained in the step (6) to obtain the tea polyphenol product of the camellia in southwest.
Preferably, in the step (2), the extraction solvent is 50% acetone-water solution, the material-to-liquid ratio (g: ml) is 1:40, the extraction temperature is 70 ℃, the extraction time is 3h, and the extraction times are 2 times.
Preferably, after adsorbing the filtrate in the step (5) by using DM130 macroporous resin, eluting impurities by using distilled water with the resin amount (ml/g) being 3 times that of the filtrate, eluting by using an ethanol solution with the resin amount (ml/g) being 13.5 times that of the filtrate and the concentration being 30%, and collecting the ethanol eluent.
The amount of the sample solution in the above step (5) was 3 times the amount of the resin (ml/g).
Further, the preparation method of the tea polyphenol in the southwest camellia comprises the following steps:
(1) pulverizing dried raw materials of the southwest camellia;
(2) refluxing and extracting the camellia southwestern in the step (1) with 50% acetone-water solution as an extraction solvent according to a material-liquid ratio (g: ml) of the camellia southwestern and the extraction solvent of 1: 40; extracting at 70 deg.C for 2 times (each for 3 hr), and mixing extractive solutions;
(3) concentrating and drying the extracting solution, dissolving in water, and filtering;
(4) adsorbing the filtrate with DM130 macroporous resin, eluting with 3 times of resin (ml/g) distilled water to remove impurities, eluting with 13.5 times of resin (ml/g) of 30% ethanol solution, collecting ethanol eluate, concentrating, and drying to obtain tea polyphenols of flos Camelliae Japonicae.
The content of tea polyphenol in the sample solution in the step (4) is 110.66 mg/ml.
Compared with the prior art, the invention has the beneficial effects that: the preparation method overcomes the defects of easy loss, low yield and low purity of tea polyphenol in the camellia sinensis in the traditional process, improves the extraction efficiency and yield of the tea polyphenol in the camellia sinensis in the southwest, effectively protects the composition, structure and activity of total polyphenol components, realizes maximum efficient production, has high purity, is simple to operate and low in cost, can recover solvents such as acetone and ethanol, can regenerate macroporous resin, and is suitable for large-scale production.
Drawings
FIG. 1: the flow chart of the preparation method of the tea polyphenol in the southwest camellia is provided in the embodiment.
Detailed Description
The present invention is further illustrated by the following specific examples, which are all developed by using phosphomolybdic tungstic acid-sodium carbonate, and the content of tea polyphenol in the camellia in southwest is determined by spectrophotometry, unless otherwise specified.
The specific implementation mode of the preparation method of the tea polyphenol in the southwest camellia flower is as follows: performing solvent extraction on dried southwest camellia flower serving as a raw material, wherein the extraction solvent is a 50-80% acetone-water solution, the material-liquid ratio (g: ml) is 1: 10-40, the extraction temperature is 60-100 ℃, the extraction time is 1-5 h, and the extraction times are 1-4 times; concentrating and drying the extract, dissolving the extract in water, filtering, adsorbing the filtrate by using DM130 macroporous resin, eluting with distilled water with the amount of resin (ml/g) being 3-5 times of that of the filtrate, eluting with an ethanol solution with the concentration of 20-60% and the amount of resin (ml/g) being 12-21 times of that of the filtrate, collecting the last part of eluent, concentrating and drying to obtain the tea polyphenol product of the camellia southwestern.
The following will describe the steps of extracting tea polyphenol and purifying resin in the southwest camellia.
First, the embodiment of the process for extracting tea polyphenol from the southwest camellia
The yield of the product tea polyphenol is calculated by the following formula:
the yield of the total polyphenol of the camellia sinense is the content of the total polyphenol of the camellia sinense multiplied by the extract content multiplied by the raw material content multiplied by 100 percent
Examples 1 to 4
The present example is to examine the effect of the concentration of the extraction solvent on the yield of tea polyphenols from camellia japonica in southwest. Specific conditions and experimental results are shown in table 1:
TABLE 1
The yield of total polyphenol is highest when the concentration of acetone is 50%, but the yield of total polyphenol is obviously reduced along with the continuous increase of the concentration of acetone, probably because the 50% acetone aqueous solution has good solubility to the total polyphenol and high swelling coefficient to raw materials. The extraction solvent was selected to be 50% acetone-water.
Examples 5 to 9
The present example is to examine the effect of extraction time on the yield of tea polyphenols in camellia japonica in southwest. Specific conditions and experimental results are shown in table 2:
TABLE 2
The total polyphenol yield is highest when the extraction time is 4 hours, and the total polyphenol yield is reduced along with the extension of the extraction time, so the optimal extraction time of 4 hours is selected.
Examples 10 to 14
The embodiment of the part inspects the influence of the extraction temperature on the yield of the tea polyphenol in the southwest camellia. Specific conditions and experimental results are shown in table 3:
TABLE 3
The total polyphenol yield increases with the increase of the extraction temperature, but the total polyphenol content obviously decreases when the temperature is higher than 70 ℃. Therefore, the optimum extraction temperature of 70 ℃ was selected.
Examples 15 to 21
The present example is to examine the effect of the feed liquid ratio on the yield of tea polyphenols in camellia japonica in southwest. Specific conditions and experimental results are shown in table 4:
TABLE 4
The yield of total polyphenols reaches the highest point when the feed-liquid ratio is 1:35, so the feed-liquid ratio is selected to be 1: 35.
Examples 22 to 25
The embodiment of the part inspects the influence of the extraction times on the yield of the tea polyphenol in the southwest camellia. Specific conditions and experimental results are shown in table 5:
TABLE 5
The yield of the total polyphenol of the camellia sinensis in southwest increases along with the increase of the extraction times, but the increasing trend is gradually reduced after more than 2 times. Considering that the energy consumption is increased by increasing the extraction times, the total polyphenol of the camellia sinense can be basically and completely extracted by 2 times of extraction. Therefore, the number of extractions was set to 2.
Example 26
This example is an orthogonal experiment for examining the extraction process, and based on the results of the previous examples 1-25, 3 levels suitable for each of the four factors were selected, and L was used9(34) The orthogonal experimental schedule examines the optimal process conditions. The orthogonal test factor level arrangement is shown in table 6, and the experimental results are shown in table 7:
TABLE 6
TABLE 7
The analysis of the experimental results shows that the influence of each factor is B>C>A>D, i.e. extraction time>Temperature of extraction>Concentration of extraction solvent>The amount of the extraction solvent is doubled; a. the2B3C1D2And A2B1C2D3The process combination is ideal, and the total polyphenol content and yield of the two combinations are relatively close, so in order to reduce the production cost of enterprises and improve the production efficiency, the optimal process combination is A2B1C2D3. Namely 40 times of 50% acetone-water, extracting for 2 times at 70 ℃, each time for 3 hours, the total polyphenol content is 41.41%, and the total polyphenol yield is 15.36%. Wherein the extraction time has a greater effect on the total polyphenol extraction.
Second, DM130 type macroporous resin purification southwest camellia flower Total Polyphenol process example
The pretreatment before use and the treatment after recovery of the DM130 macroporous resin comprise the following specific pretreatment steps: adding ethanol 10-20cm higher than the resin layer into the extractor, soaking for 2-4 hr, and washing with washing solution. Repeatedly washing with the same method until the outlet washing solution is not turbid after adding 3 times of water in the test tube, and then sufficiently rinsing with distilled water until no obvious ethanol smell exists.
In order to optimize the use of resin, the present embodiment first examines the performance parameters of the resin, and the specific procedures are as follows:
1. determination of dynamic adsorption quantity
And (3) loading 20g of DM130 type macroporous adsorption resin into a column (the diameter-height ratio is 1: 10), continuously passing the sample solution through the resin column at the flow rate of 2BV/h, collecting effluent, determining the concentration of the total polyphenol of the camellia southwestern in the effluent, and drawing an adsorption curve by taking the concentration (mg/mL) of the total polyphenol of the camellia southwestern in the effluent as an ordinate and the volume (mL) of the sample solution as an abscissa. The results are shown in Table 8, and when the volume of the sample solution is increased to 210mL, the DM130 macroporous adsorbent resin is saturated.
TABLE 8 dynamic adsorption of the Total polyphenols from Camellia sinensis in southwest
2. Determination of static adsorption quantity
A100 mL Erlenmeyer flask was charged with 10mL (about 3g dry resin equivalent) of the pretreated DM130 type macroporous adsorbent resin and 100mL of sample solution. Oscillating at room temperature for 3 hours, taking out and measuring the content of the total polyphenol of the southwestern camellia in the sample solution, and calculating the static adsorption capacity q ═ C (C) in material balance according to the following formula0C) V/G, the static adsorption capacity of DM130 macroporous resin is found to be 87.0mg polyphenol per G macroporous resin, wherein C0And C is the concentration (mg/mL) of the total polyphenol of the southwestern camellia in the solution at the initial stage and the equilibrium stage respectively, V is the volume (mL) of the test solution, and G is the resin amount (G).
Examples 27 to 31
In this section, ethanol elution concentration of DM130 macroporous resin is examined. Specific conditions and experimental results are shown in table 9:
TABLE 9
The purity and elution rate of total polyphenol are reduced along with the increase of the concentration of ethanol, and 30% ethanol is selected for elution in order to improve the content and elution rate of the total polyphenol. As a result, the total polyphenol content and the elution rate are respectively improved to 85.27 percent and 21.91 percent. The results show that the purity and elution rate of the total polyphenol are improved by using water and 30 percent ethanol for elution.
Examples 32 to 40
The present example considers the amount of eluent of DM130 type macroporous adsorption resin. Specific conditions and experimental results are shown in table 10:
watch 10
Deionized water 3 times the weight of the resin can be used for basically removing water-soluble impurities, and 30% ethanol elution 13.5 times the weight of the resin can be used for basically completely eluting the total polyphenol, so that the use amount of the deionized water is determined to be 3 times the weight of the resin, and the use amount of the 30% ethanol elution is determined to be 13.5 times the weight of the resin.
EXAMPLE 41
The process flow of the embodiment is shown in the attached figure 1
1. Pulverizing dried raw materials of the southwest camellia;
2. extracting with 50% acetone-water solution at 70 deg.C at a ratio of 1:40 (g: ml) for 2 times (3 hr each time);
3. concentrating and drying the extract, dissolving in water, and filtering to obtain a total polyphenol content of 41.41%;
4. adsorbing the filtrate by using DM130 macroporous resin, wherein the sample loading amount is 3 times of the resin amount (ml/g), eluting with distilled water with the resin amount (ml/g) being 3 times of the resin amount (ml/g), eluting with an ethanol solution with the concentration of 30% and 13.5 times of the resin amount (ml/g), collecting the last part of eluent, concentrating and drying to obtain a tea polyphenol product of the camellia sinense, wherein the purity of the obtained total polyphenol is 85.27%.
Claims (6)
1. The preparation method of the tea polyphenol in the southwest camellia is characterized by comprising the following steps:
(1) pulverizing dried raw materials of the southwest camellia;
(2) refluxing and extracting the camellia southwestern in the step (1) by taking 50-80% acetone-water solution as a solvent and taking the ratio (g: ml) of the camellia southwestern and the extraction solvent as 1: 10-40; extracting at the temperature of 60-100 ℃ for 1-5 h for 1-4 times, and combining the extracting solutions;
(3) screening out the extract with the highest total polyphenol yield through a single-factor experiment and an orthogonal experiment;
(4) concentrating and drying the extracting solution in the step (3), dissolving in water, and filtering;
(5) adsorbing the filtrate by using DM130 macroporous resin, eluting impurities by using distilled water with the resin amount (ml/g) being 3-5 times of that of the filtrate, eluting the impurities completely by using an ethanol solution with the concentration of 20-60% and the resin amount (ml/g) being 12-21 times of that of the filtrate, and collecting the eluent;
(6) screening the eluent with the highest total polyphenol content through a single-factor experiment;
(7) and (4) concentrating and drying the eluent obtained in the step (6) to obtain the tea polyphenol product of the camellia in southwest.
2. The method for preparing tea polyphenols from camellia japonica thunb as claimed in claim 1, wherein the extraction solvent is 50% acetone-water solution, the ratio of the raw materials to the liquid (g: ml) is 1:40, the extraction temperature is 70 ℃, the extraction time is 3h, and the extraction times are 2 times.
3. The method for preparing tea polyphenols from camellia japonica thunb as claimed in claim 1, wherein the filtrate obtained in step (5) is adsorbed by DM130 macroporous resin, and then eluted with distilled water 3 times the resin amount (ml/g) and then eluted with 30% ethanol solution 13.5 times the resin amount (ml/g), and the ethanol eluate is collected.
4. The method for preparing tea polyphenols from camellia japonica thunb as claimed in claim 3, wherein the amount of the loading solution in step (5) is 3 times the amount of the resin (ml/g).
5. The method for producing tea polyphenols from camellia sinensis as claimed in claim 1, wherein the method comprises the following steps:
(1) pulverizing dried raw materials of the southwest camellia;
(2) refluxing and extracting the camellia southwestern in the step (1) with 50% acetone-water solution as an extraction solvent according to a material-liquid ratio (g: ml) of the camellia southwestern and the extraction solvent of 1: 40; extracting at 70 deg.C for 2 times (each for 3 hr), and mixing extractive solutions;
(3) concentrating and drying the extracting solution, dissolving in water, and filtering;
(4) adsorbing the filtrate with DM130 macroporous resin, eluting with 3 times of resin (ml/g) distilled water to remove impurities, eluting with 13.5 times of resin (ml/g) of 30% ethanol solution, collecting ethanol eluate, concentrating, and drying to obtain tea polyphenols of flos Camelliae Japonicae.
6. The method for preparing tea polyphenols from camellia japonica thunb as claimed in claim 5, wherein the content of tea polyphenols in the sample solution in the step (4) is 110.66 mg/ml.
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| CN103145770A (en) * | 2013-03-20 | 2013-06-12 | 宜宾学院 | Method for extracting polyphenol from camellia |
| CN106478744A (en) * | 2016-08-26 | 2017-03-08 | 潜山县妙山茶业有限公司 | A kind of technique extracting tea polyphenols from Folium Camelliae sinensis |
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|---|---|---|---|---|
| CN103145770A (en) * | 2013-03-20 | 2013-06-12 | 宜宾学院 | Method for extracting polyphenol from camellia |
| CN106478744A (en) * | 2016-08-26 | 2017-03-08 | 潜山县妙山茶业有限公司 | A kind of technique extracting tea polyphenols from Folium Camelliae sinensis |
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| 不同提取方法对茶多酚理化性质的影响;蒋丽等;《食品科学》;20100715;第31卷(第14期);第139页表1 * |
| 西南山茶植物不同部位化学成分的定量分析;侯蕾等;《华西药学杂志》;20100215;第25卷(第01期);第40-43页 * |
| 西南山茶花化学成分的定量分析;侯蕾等;《云南中医学院学报》;20100420;第33卷(第02期);第25-28页 * |
| 西南红山茶花化学成分的分离与鉴定;候蕾等;《时珍国医国药》;20110720;第22卷(第7期);第1701页摘要第2-5行 * |
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