CN101108842A - Process technique for extracting tea polyphenol from tree plant flower - Google Patents
Process technique for extracting tea polyphenol from tree plant flower Download PDFInfo
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Abstract
A process technology extracting the tea polyphenols from the tea plant flowers is provided, which relates to the preparation technology of the separation and purification of the tea polyphenols. The process technology comprises the following steps: 1) drying the tea tree pollen; 2) producing the extracting solution by ultrasonic wave; 3) producing ultrafiltration treatment filter liquor after extraction, condensation, microfiltration and ultrafiltration; 4) gaining polyphenols extracting solution through absorption by medium polarity adsorbent resins; 5) producing the extracting solution to the extract and producing the extract to the polyphenol fine powder of the tea plant flowers. Compared with the method using the current tea to prepare tea polyphenols, the invention has the following advantages that aiming at the characteristics of abundant content of the polyphenols of the tea plant flowers, little pigment impurity and good stability, the invention carries out the comprehensive development and use to change waste into valuable, replaces the tea leaves to extract the natural tea polyphenols and provides raw materials and additives with high quality for the industries such as medicine, food and cosmetic. The invention improves the utilization rate of the tea plant flowers resources and is suitable for the scale production, reduces the energy consumption and production cost and enhances the competitiveness of the production.
Description
Technical field
The present invention relates to the preparation technology of tea tree, the separation and purification of tealeaves polyphenol, it belongs to the deep processing art of natural organic chemistry field and agricultural-food, relates in particular to the preparation technology of ultrasonic wave-ultrafiltration-macroporous adsorbent resin coupling separation and purification target components.
Background technology
Tea tree contains similar to the bright leaf of tea such as multiple natural constituents such as tea-polyphenol, protein, polysaccharide, wherein the tea-polyphenol based on catechin has the human free radical of removing and improves immunizing power, effects such as anti-oxidant, anti-ageing, radioprotective, reducing blood-fat, fat-reducing, medicine, healthcare products, makeup and food service industry have been widely used in, it is the natural active substance of safety, application prospect is boundless, but its natural resources is limited, mostly is from tealeaves at present and extracts.Tea tree is the reproductive organ of tea tree, from blooming to the result, needs 17 months, and the nutrition that has consumed tea tree influences tea yield, quality, and the tea grower usually buries its pruning for improving tea yield, quality, and a large amount of tea tree perianth is discarded.Utilize depleted tea tree resource, it is more more economical than tealeaves therefrom to extract natural antioxidants, and this greatly reduces the extraction cost of tea-polyphenol, and the natural polyphenol of having opened up resource shortage obtains new way.Improve the tea grower simultaneously and plant the tea economy benefit, rich worker rich peasant has greatly comprehensive social benefit.
What extract tea-polyphenol employing at present from tealeaves mainly is solvent-extraction process (comprising water and water-containing organic solvent), the heavy metallic salt precipitator method and resin absorption concentration method.Solvent-extraction process will remove pigment and caffeine with chloroform extraction filtrate; The precipitation rule adopts tea-polyphenol in the heavy metal ion precipitation filtrate, and it is separated with caffeine with pigment, and these two kinds of methods may cause organic solvent or the heavy-metal residual in the tea-polyphenol product, and the tea-polyphenol purity of preparation is not high.Method by thick tea-polyphenol separation and Extraction catechin has supercritical CO
2Extraction process, this method product purity is higher, but complex process, it is single to separate component, operation inconvenience, cost height; Liquid phantom preparing chromatogram and counter current chromatography, the tea polyphenol monomer isolate purity height of preparation, recovering effect is better, but the cost of investment height, and throughput is " gram magnitude ", is difficult to the expansion scale.
Summary of the invention
The object of the present invention is to provide a kind of is raw material with the tea tree, adopts the technology of ultrasonic wave-ultrafiltration-macroporous adsorbent resin coupling, extracts the complete processing of tea-polyphenol from tea tree.
Technical scheme of the present invention may further comprise the steps:
1), fresh tea tree spends drying, makes dried tea tree, and pulverizing;
2), will to spend end and concentration in container be that 60% ethanol mixes according to 1: 20～25 weight ratio, left standstill 4～9 hours, inserts then in the ultrasonic wave lixiviate still, is heated to 50～60 ℃, insulation 20～30min takes out filtration, gets extracting solution;
3), extracting solution is inserted vacuum concentrating apparatus, reclaim ethanol, when extracting liquid volume is reduced to 1/5～1/3 in the container, stop to take out, in container, add entry to original volume; Carry out micro-filtration, carry out ultrafiltration behind the micro-filtration, select for use MWCO at 50,000～100,000 ultra-filtration membranes, at normal temperatures, ultrafiltration pressure is 0.10～0.30MPa, and to proceed to feed liquid surplus 10～20% the time when ultrafiltration, adds the water dialysis at least once, makes tea-polyphenol uf processing filtrate;
4), adopt the middle polarity polymeric adsorbent, with its wet method resin column of packing into, after the water washing balance, the tea tree flower polyphenol uf processing filtrate of last step is added resin column adsorb, detect and spill liquid polyphenol concentration and reach 10 of initial upper prop concentration～20% and o'clock stop upper prop; With the distilled water of 2～3 times of resin column volumes or pH value is 2.0～3.0 the quick drip washing of 5～10% aqueous ethanolic solutions, impurity such as flush away oligosaccharides, pigment, trimethyl-xanthine; The tea tree flower polyphenol adopts 30～70% ethanol liquid gradient elution resin layers of 3 times of resin column volumes, collects elutriant, gets the polyphenol extracting solution;
5), the polyphenol extracting solution is inserted vacuum concentrating apparatus, reclaim ethanol, medicinal extract, with extract dry, make the smart powder of tea tree flower polyphenol.
The fresh tea tree flower of gathering in the scene carries out 60～80 ℃ of vacuum dehydrating at lower temperature or a formula drying; The dry gradient temperature that adopts of bed formula is dried, and bake out temperature is 70～120 ℃, makes dried tea tree water content below 8%; Again dried tea tree is pulverized with pulverizer, be crushed to 30～60 orders.
To proceed to feed liquid surplus 15～20% the time when ultrafiltration, adds water dialysis 2～5 times, and each amount of water is 4～6 times of former dried flower quality.
The middle polarity polymeric adsorbent is YZ-806, HZ-816, NKA-9, B4, Amberlite XAD-7, HP-20.
The polyphenol extracting solution is carried out vacuum concentration reclaim ethanol, extracting liquid volume is reduced to 1/3 when following of original volume, takes out, and spissated extracting solution vacuum-drying, spraying drying or vacuum lyophilization make high purity tea tree flower polyphenol essence powder.
The resin of wash-out tea-polyphenol is used the alkali of 2～5% concentration of 2 times of resin column volumes and acid, 95% washing with alcohol respectively, recovers the resin absorption ability.
Among the present invention, the lixiviate of ultrasonic wave secondary solvent can guarantee that to greatest extent tea-polyphenol effective constituent is not destroyed at low temperature effective lixiviate tea-polyphenol in the short period of time, and its leaching yield is higher than conventional solvent lixiviate.Conventional solvent extraction time is long, the temperature height, and the polyphenol destructible, efficient is low, and running cost is big.
The ultra-filtration membrane sepn process does not undergo phase transition, and separation of material heating or refrigerative energy consumption are very low; Usually can carry out at normal temperatures, be particularly suitable for separation, the classification of heat-sensitive substance, help keeping biological activity, the physical and chemical stability height of product, loss of active ingredients significantly reduces; The scale of sepn process and processing power can in very large range change, and convenient the adjustment, and equipment unit price, working cost are low.
The macroporous adsorbent resin of middle polarity is novel non-ionic type molecular adsorption medium, has demonstrated the centrifugation of its uniqueness.This method is to utilize the molecular sieve and the adsorption property of polymeric adsorbent, makes catechin adsorption-desorption and other separating substances on polymeric adsorbent, and reaches the separation and purification purpose.Adopt gradient elution can obtain the different polyphenol products of forming of high purity.Adsorption resin method is easy and simple to handle, and resin is also renewable to be used repeatedly, and stability is high, and cost is low, easily moves towards the industrialization.But use the macroporous adsorbent resin technology to exist the purity of product not high enough separately, resin is easily by the defective of contaminating impurity.
The present invention compares with existing preparation of tea tea-polyphenol method has following advantage, abundant at tea tree flower polyphenol content, pigment impurity is few, the characteristics of good stability, carry out comprehensive development and utilization, turn waste into wealth, replace tealeaves to extract natural tea polyphenol, for industries such as medicine, food, makeup provide high-quality raw material, additive.This technical process can guarantee that to greatest extent tea-polyphenol effective constituent is not destroyed at low temperature transitory efficient rate lixiviate tea-polyphenol by the lixiviate of ultrasonic wave secondary solvent.Macromolecular substance such as the protein in the ultrafiltration removal extracting solution, polysaccharide, owing to removed partial impurities, macroporous adsorbent resin has been obtained good solution by the problem of contaminating impurity easily, the separation and purification better effects if.Whole technology is not introduced other organic solvents and chemical substance except that edible ethanol, making product is that pure natural refines product, safe and reliable, making whole process of production not have any environmental pollution, is that other separation methods can't be compared, and makes the development and use of this project have more reasonableness.The present invention has improved the tea tree resource utilization, adapts to large-scale production, reduces energy consumption and production costs, and strengthens the competitive power of producing.
Embodiment
Embodiment 1
The fresh tea tree flower of gathering in the scene makes dried tea tree by low-temperature vacuum drying, reduces the oxidational losses of polyphenol in preserving process.The broken machine of tea plant pollen is crushed to about 50 orders, and 3kg pulverizes tea tree and mixes with 60 L60% ethanol, behind the cold soaking 8h, in the ultrasonic extraction equipment of the temperature control of packing into, is heated to 55 ℃, and ultrasonic extraction 20min filters; Extract adding 30 L60% ethanol for the second time, be heated to 55 ℃, ultrasonic extraction 5min filters.Merge filtrate twice.The filtrate vacuum concentration reclaims ethanol, reduces extracting solution ethanol volume fraction, adds water and complements to 100L.Micro-filtration clarification tea tree vat liquor is removed feed liquid and is included a large amount of tea tree fine particle, suspended impurity, alleviates the pollution to follow-up ultra-filtration membrane, gets clarifying tea tree extracting solution 100L, contains tea tree flower polyphenol 221.2120g.
The 100L extracting solution pumped into carry out ultrafiltration in the ultrafiltration apparatus, remove protein, tea polysaccharide, pectin or the like impurity, collect ultrafiltrated.Select PS material polysulfone hollow fiber ultrafiltration membrane system for use, MWCO is 50,000.The ultrafiltration technology condition is: 30 ℃ of service temperatures, ultrafiltration pressure 0.10MPa.When ultrafiltration proceeds to the surplus 15L of feed liquid, add 15L water dialysis twice, collect the about 115L of ultrafiltrated, contain tea tree flower polyphenol 180.3525g, the polyphenol extraction yield is 81.53%.
The Semi-polarity macroporous adsorbent resin YZ-806 wet method resin column of packing into screening, after the water washing balance, with the optimal adsorption condition: go up column liquid concentration 1mg/ml, upper prop liquid pH3.0, last column flow rate 4BV/h (BV is the resin column volume) pumps into resin column with tea tree flower polyphenol ultrafiltrated and adsorbs, and detects to spill liquid polyphenol concentration and reach 15% o'clock of starting point concentration and stop upper prop; With the quick drip washing of 3BV distilled water, impurity such as flush away oligosaccharides, pigment; The tea tree flower polyphenol adopts 30～70 ℃ of ethanol liquid of 3BV with the gradient elution resin layer, collects elutriant.Elutriant contains tea tree flower polyphenol 152.9930g, and the polyphenol adsorption rate is 86.39%, desorption efficiency 98.20%.
Elutriant carries out rotary evaporation in vacuo and reclaims ethanol, and vacuum lyophilization obtains tea tree flower polyphenol product 181.4433g.
Whole technology tea tree flower polyphenol extraction yield is about 67.8%, and yield is about 5.1%.Tea tree flower polyphenol purity 84.32%, total catechin content 65.02%, wherein EGCG content 28.87%.
Embodiment 2
The fresh tea tree flower of gathering in the scene makes dried tea tree by low-temperature vacuum drying, reduces the oxidational losses of polyphenol in preserving process.The broken machine of tea plant pollen is crushed to about 50 orders, and 3kg pulverizes tea tree and mixes with 70 L60% ethanol, behind cold soaking 4 h, in the ultrasonic extraction equipment of the temperature control of packing into, is heated to 60 ℃, and ultrasonic extraction 30min filters; Extract adding 30 L60% ethanol for the second time, be heated to 60 ℃, ultrasonic extraction 5min filters.Merge filtrate twice.The filtrate vacuum concentration reclaims ethanol, reduces extracting solution ethanol volume fraction, adds water and complements to 100L.Micro-filtration clarification tea tree vat liquor is removed feed liquid and is included a large amount of tea tree fine particle, suspended impurity, alleviates the pollution to follow-up ultra-filtration membrane, gets clarifying tea tree extracting solution 100L, contains tea tree flower polyphenol 225.0214g.
The 100L extracting solution pumped into carry out ultrafiltration in the ultrafiltration apparatus, remove protein, tea polysaccharide, pectin or the like impurity, collect ultrafiltrated.Select polyetherketone material flat plate ultrafiltration membrane assembly for use, MWCO is 70,000.The ultrafiltration technology condition is: 30 ℃ of service temperatures, ultrafiltration pressure 0.10MPa.When ultrafiltration proceeds to the surplus 10L of feed liquid, add 10L water dialysis twice, collect the about 110L of ultrafiltrated, contain tea tree flower polyphenol 200.7190g, the polyphenol extraction yield is 89.23%.
The Semi-polarity macroporous adsorbent resin HZ-816 wet method resin column of packing into screening, after the water washing balance, with the optimal adsorption condition: go up column liquid concentration 1mg/ml, upper prop liquid pH 2.5, last column flow rate 4BV/h (BV is the resin column volume) pumps into resin column with tea tree flower polyphenol ultrafiltrated and adsorbs, and detects to spill to stop upper prop when liquid polyphenol concentration reaches starting point concentration 20%; With the quick drip washing of 3BV distilled water, impurity such as flush away oligosaccharides, pigment; The tea tree flower polyphenol adopts 30～70 ℃ of ethanol liquid of 3BV with the gradient elution resin layer, collects elutriant.Elutriant contains tea tree flower polyphenol 159.8490g, and the polyphenol adsorption rate is 80.24%, desorption efficiency 99.25%.
Elutriant carries out rotary evaporation in vacuo and reclaims ethanol, and vacuum lyophilization obtains tea tree flower polyphenol product 193.0310g.
Whole technology tea tree flower polyphenol extraction yield is about 71.0%, and yield is about 5.3%.Tea tree flower polyphenol purity 82.81%, total catechin content 63.47%, wherein EGCG content 28.20%.
Embodiment 3
The fresh tea tree flower of gathering in the scene makes dried tea tree by low-temperature vacuum drying, reduces the oxidational losses of polyphenol in preserving process.The broken machine of tea plant pollen is crushed to about 50 orders, and 3kg pulverizes tea tree and mixes with 75L60% ethanol, behind the cold soaking 9h, in the ultrasonic extraction equipment of the temperature control of packing into, is heated to 50 ℃, and ultrasonic extraction 25min filters; Extract adding 30 L60% ethanol for the second time, be heated to 50 ℃, ultrasonic extraction 5min filters.Merge filtrate twice.The filtrate vacuum concentration reclaims ethanol, reduces extracting solution ethanol volume fraction, adds water and complements to 100L.Micro-filtration clarification tea tree vat liquor is removed feed liquid and is included a large amount of tea tree fine particle, suspended impurity, alleviates the pollution to follow-up ultra-filtration membrane, gets clarifying tea tree extracting solution 100L, contains tea tree flower polyphenol 222.8010g.
The 100L extracting solution pumped into carry out ultrafiltration in the ultrafiltration apparatus, remove protein, tea polysaccharide, pectin or the like impurity, collect ultrafiltrated.Select PVDF material polysulfone hollow fiber ultrafiltration membrane system for use, MWCO is 100,000.The ultrafiltration technology condition is: 30 ℃ of service temperatures, ultrafiltration pressure 0.08MPa.When ultrafiltration proceeds to the surplus 20L of feed liquid, add 20L water dialysis twice, collect the about 120L of ultrafiltrated, contain tea tree flower polyphenol 205.1997g, the polyphenol extraction yield is 92.15%.
The Semi-polarity macroporous adsorbent resin HP-20 wet method resin column of packing into screening, after the water washing balance, with the optimal adsorption condition: go up column liquid concentration 1mg/ml, upper prop liquid pH 2.0, last column flow rate 4BV/h (BV is the resin column volume) pumps into resin column with tea tree flower polyphenol ultrafiltrated and adsorbs, and detects to spill liquid polyphenol concentration and reach 10% o'clock of starting point concentration and stop upper prop; With the quick drip washing of 3BV distilled water, impurity such as flush away oligosaccharides, pigment; The tea tree flower polyphenol adopts 30～70 ℃ of ethanol liquid of 4BV with the gradient elution resin layer, collects elutriant.Elutriant contains tea tree flower polyphenol 194.8140g, and the polyphenol adsorption rate is 92.06%, desorption efficiency 94.98%.
Elutriant carries out rotary evaporation in vacuo and reclaims ethanol, and vacuum lyophilization obtains tea tree flower polyphenol product 228.1729g.
Whole technology tea tree flower polyphenol extraction yield is about 79.7%, and yield is about 6.5%.Tea tree flower polyphenol purity 85.38%, total catechin content 65.98%, wherein EGCG content 28.92%.
Claims (6)
1. complete processing of extracting tea-polyphenol from tea tree is characterized in that it may further comprise the steps:
1), fresh tea tree spends drying, makes dried tea tree, and pulverizing;
2), will to spend end and concentration in container be that 60% ethanol mixes according to 1: 20～25 weight ratio, left standstill 4～9 hours, inserts then in the ultrasonic wave lixiviate still, is heated to 50～60 ℃, insulation 20～30min takes out filtration, gets extracting solution;
3), extracting solution is inserted vacuum concentrating apparatus, reclaim ethanol, when extracting liquid volume is reduced to 1/5～1/3 in the container, stop to take out, in container, add entry to original volume; Carry out micro-filtration, carry out ultrafiltration behind the micro-filtration, select for use MWCO at 50,000～100,000 ultra-filtration membranes, at normal temperatures, ultrafiltration pressure is 0.10～0.30MPa, and to proceed to feed liquid surplus 10～20% the time when ultrafiltration, adds the water dialysis at least once, makes tea-polyphenol uf processing filtrate;
4), adopt the middle polarity polymeric adsorbent, with its wet method resin column of packing into, after the water washing balance, the tea tree flower polyphenol uf processing filtrate of last step is added resin column adsorb, detect and spill liquid polyphenol concentration and reach 10 of initial upper prop concentration～20% and o'clock stop upper prop; With the distilled water of 2～3 times of resin column volumes or pH value is 2.0～3.0 the quick drip washing of 5～10% aqueous ethanolic solutions, impurity such as flush away oligosaccharides, pigment, trimethyl-xanthine; The tea tree flower polyphenol adopts 30～70% ethanol liquid gradient elution resin layers of 3 times of resin column volumes, collects elutriant, gets the polyphenol extracting solution;
5), the polyphenol extracting solution is inserted vacuum concentrating apparatus, reclaim ethanol, medicinal extract, with extract dry, make the smart powder of tea tree flower polyphenol.
2. the complete processing of extracting tea-polyphenol from tea tree as claimed in claim 1 is characterized in that, the fresh tea tree flower of gathering in the scene carries out 60～80 ℃ of vacuum dehydrating at lower temperature or a formula drying; The dry gradient temperature that adopts of bed formula is dried, and bake out temperature is 70～120 ℃, makes dried tea tree water content below 8%; Again dried tea tree is pulverized with pulverizer, be crushed to 30～60 orders.
3. a kind of complete processing of extracting tea-polyphenol from tea tree as claimed in claim 1 is characterized in that, to proceed to feed liquid surplus 15～20% the time when ultrafiltration, adds water dialysis 2～5 times, and each amount of water is 4～6 times of former dried flower quality.
4. the complete processing of extracting tea-polyphenol from tea tree as claimed in claim 1 is characterized in that the middle polarity polymeric adsorbent is YZ-806, HZ-816, NKA-9, B4, Amberlite XAD-7, HP-20.
5. the complete processing of from tea tree, extracting tea-polyphenol as claimed in claim 1, it is characterized in that, the polyphenol extracting solution is carried out vacuum concentration reclaim ethanol, extracting liquid volume is reduced to 1/3 when following of original volume, take out, spissated extracting solution vacuum-drying, spraying drying or vacuum lyophilization make the smart powder of high purity tea tree flower polyphenol.
6. the complete processing of extracting tea-polyphenol from tea tree as claimed in claim 1 is characterized in that, the resin of wash-out tea-polyphenol is used the alkali of 2～5% concentration of 2 times of resin column volumes and acid, 95% washing with alcohol respectively, recovers the resin absorption ability.
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| CN109394617A (en) * | 2018-11-21 | 2019-03-01 | 广西壮族自治区林业科学研究院 | A method of tea polyphenols are extracted using Camellia Leaves and prepare natural hand cleanser |
| CN109620788A (en) * | 2019-01-30 | 2019-04-16 | 周忠平 | A kind of process for extracting tea polyphenol and its application in beautifying whitening liquid |
| CN109673781A (en) * | 2019-02-27 | 2019-04-26 | 厦门元之道生物科技有限公司 | A kind of active polyphenol fermentation liquid of high anti-oxidation and its preparation process |
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