CN103815078A - Method for extracting low-caffeine low-content tea polyphenol from fresh tea - Google Patents

Method for extracting low-caffeine low-content tea polyphenol from fresh tea Download PDF

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CN103815078A
CN103815078A CN201410067192.8A CN201410067192A CN103815078A CN 103815078 A CN103815078 A CN 103815078A CN 201410067192 A CN201410067192 A CN 201410067192A CN 103815078 A CN103815078 A CN 103815078A
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tea
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顾峰
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CHENGDU WAGOTT BIO-TECH Co Ltd
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Abstract

The invention discloses a method for extracting low-caffeine low-content tea polyphenol from fresh tea, belonging to the technical field of chemistry of natural products. The method comprises the following concrete steps: S1, soaking; S2, centrifugation; S3, resin adsorption; S4, membrane concentration; S5, evaporative concentration; S6, spray drying; and S7, deironing. According to the invention, fresh tea is used as a raw material; the disadvantages of easy pasting and uneasy filtration during extraction of crushed and sieved dry tea at a high temperature in the prior art is overcome; purified water is used as a medium for direct separation of low-caffeine low-content tea polyphenol, and leaching of a plurality of fat-soluble pesticides is reduced; after extraction, the obtained product has tea polyphenol content of lower than 50% and caffeine content of lower than 1%. The method has the advantages of simple operation, high separation efficiency, low cost and a short production period and is suitable for industrialized large-scale production.

Description

A kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its
Technical field
The invention belongs to natural product chemistry technical field, be specifically related to a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its.
Background technology
Tea Polyphenols (Tea polyphenols, TP) is a kind of new type natural antioxidant extracting from tealeaves, has a series of important pharmacological functions such as anticancer, anti-ageing, radioresistance, removing human free radical, hypoglycemic blood fat.Have broad application prospects in fields such as grease, food, medicine, daily use chemicals.Tea Polyphenols is the mixture of multiple catechin monomers, wherein having active component anti-oxidant, anticancer and removing interior free yl is nutgall catechin gallic acid ester (epigallocatechin gallate, EGCG), it by universally acknowledged for being " the optimal cancer therapy drug extracting from natural plants after taxol ".In October, 2006, food and drug administration (FDA) approval Tea Polyphenols, as new prescription medicine, treats for local (outside) genital wart being caused by human papilloma virus.This is that FDA is according to first plant (draft) medicine of medicine amendment regulations approval listing in 1962.
Caffeine (having another name called caffeine) formal name used at school is 1,3,7-trimethyl-2, and 6 dioxypurines have stimulating central nervous system, eliminate the functions such as fatigue, diuresis, relaxing smooth muscle and cardiac stimulant solution contraction.In tealeaves, conventionally contain 2%-5% caffeine, appropriate absorption caffeine is harmless to normal adults, but some old men, pregnant woman, children, cardiac dysfunction and neurastheniac, after drinking tea, tend to produce some to health or the disadvantageous side effect of offspring, short time excessive use caffeine, may cause some people's lather, insomnia, headache and palpitaition; In addition, have tea too much or drink strong tea, often impact sleep at night.
Low-caffeine low content Tea Polyphenols refers to content≤1% of caffeine in product, the content <50% of Tea Polyphenols, it is high that low-caffeine low content Tea Polyphenols has clarity, dissolubility is good, the features such as bitter taste is low, caffeine is low, be applicable to food beverage industry, also can for old, in, few consumers in general colony.
Tea Polyphenols purity height, particularly caffeine and catechin content have directly determined quality and the purposes of product.Therefore, prepare low-caffeine low content Tea Polyphenols and become the technical barrier that this area urgently need solve at present.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its is provided, that this method has advantages of is simple to operate, separative efficiency is high, cost is low, with short production cycle.
Object of the present invention is achieved through the following technical solutions: a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its, and it comprises the following steps:
S1. soak: fresh tea leaf in its is placed in to digester, adds purified water constant temperature to soak 1.8~2.5h, the mixed liquor in digester is crossed to 18~24 mesh sieves, obtain filtrate; Wherein, described constant temperature soaking temperature is 65~100 ℃;
S2. centrifugal: it is centrifugal 50~70s under 30~50 ℃, the pressure environment that is 0.2~0.4MPa that filtrate is placed in to temperature, discards precipitation, and centrifugate is for next-step operation; Wherein, the rotating speed of described centrifuge is 6500~7000 turn/min;
S3. resin adsorption: centrifugate is splined on to HZ818 resin, the caffeine in absorption filtrate, the efflux that collection solid content is 2.5~3.5%;
S4. film is concentrated: the efflux that the reverse osmosis membrane concentration step S3 that employing molecular cut off is 100 collects, is concentrated into solid content >=20%;
S5. evaporation and concentration: concentrate is heated to temperature >=75 ℃, and evaporation and concentration to solid content is 40~50%, is cooled to normal temperature;
S6. spraying is dry: the concentrate that step S5 evaporation and concentration is crossed is sprayed dry, controls 75~100 ℃ of 160~220 ℃ of EATs, leaving air temps, the feed pressure 15~20MPa of spray dryer;
S7. deironing: dry spraying gained solid is pulverized with pulverizer, crossed 50~90 mesh sieves, use magnet adsorption deironing, after deironing, powder is mixed, again sieve, magnet adsorption deironing, make low-caffeine low content Tea Polyphenols.
Further, the weight ratio of fresh tea leaf in its and purified water described in step S1 is 1:5~8.
Further, elution speed described in step S3 is 1.8~2.4m 3/ h.
Further, the magnetic force of magnet described in step S7 is 10000~15000 Gausses.
The present invention has the following advantages: it is raw material that the present invention adopts fresh tea leaf in its, easy gelatinization while having overcome at high temperature lixiviate after adopting stem tea to pulverize and sieve in traditional handicraft, is difficult for the shortcoming of filtering; Do medium with purified water and directly isolate low-caffeine low content Tea Polyphenols, reduced the leaching of some fat-soluble agricultural chemicals; Product after extracting can make polyphenol content lower than 50%, and content of caffeine is lower than 1%.The low-caffeine low content Tea Polyphenols appearance luster brown color that adopts the inventive method to prepare, is instant product, and water-soluble rear clarity of solution is high, and soup look Huang is bright, low bitter taste.That this method has is simple to operate, separative efficiency is high, cost is low, with short production cycle, be applicable to batch production large-scale production.
The specific embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated.
Embodiment 1: a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its, it comprises the following steps:
S1. soak: fresh tea leaf in its 2000kg is placed in to digester, adds purified water 10000kg, constant temperature soaks 1.8h, and the mixed liquor in digester is crossed to 18 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 65 ℃;
S2. centrifugal: it is centrifugal 50s under 30 ℃, the pressure environment that is 0.2MPa that filtrate is placed in to temperature, discards precipitation, and centrifugate is for next-step operation; Wherein, the rotating speed of described centrifuge is 6500 turn/min;
S3. resin adsorption: centrifugate is splined on to HZ818 resin, and elution speed is 1.8m 3/ h, the caffeine in absorption filtrate, the efflux that collection solid content is 2.5%;
S4. film is concentrated: the efflux that the reverse osmosis membrane concentration step S3 that employing molecular cut off is 100 collects, and being concentrated into solid content is 20%;
S5. evaporation and concentration: concentrate is heated to 75 ℃, and evaporation and concentration to solid content is 40%, is cooled to normal temperature;
S6. spraying is dry: the concentrate that step S5 evaporation and concentration is crossed is sprayed dry, controls 75 ℃ of 160 ℃ of EATs, leaving air temps, the feed pressure 15MPa of spray dryer;
S7. deironing: dry spraying gained solid is pulverized with pulverizer, cross 50 mesh sieves, it is 10000 Gausses' magnet adsorption deironing with magnetic force, after deironing, powder is mixed, again sieve, magnet adsorption deironing, make low-caffeine low content Tea Polyphenols 22kg, in product, content of caffeine is 0.12%, and polyphenol content is 47.5%.
Embodiment 2: a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its, it comprises the following steps:
S1. soak: fresh tea leaf in its 2000kg is placed in to digester, adds purified water 16000kg, constant temperature soaks 2.5h, and the mixed liquor in digester is crossed to 24 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 100 ℃;
S2. centrifugal: it is centrifugal 70s under 50 ℃, the pressure environment that is 0.4MPa that filtrate is placed in to temperature, discards precipitation, and centrifugate is for next-step operation; Wherein, the rotating speed of described centrifuge is 7000 turn/min;
S3. resin adsorption: centrifugate is splined on to HZ818 resin, and elution speed is 2.4m 3/ h, the caffeine in absorption filtrate, the efflux that collection solid content is 3.5%;
S4. film is concentrated: the efflux that the reverse osmosis membrane concentration step S3 that employing molecular cut off is 100 collects, and being concentrated into solid content is 30%;
S5. evaporation and concentration: concentrate is heated to 85 ℃, and evaporation and concentration to solid content is 60%, is cooled to normal temperature;
S6. spraying is dry: the concentrate that step S5 evaporation and concentration is crossed is sprayed dry, controls 100 ℃ of 220 ℃ of EATs, leaving air temps, the feed pressure 20MPa of spray dryer;
S7. deironing: dry spraying gained solid is pulverized with pulverizer, cross 90 mesh sieves, it is 15000 Gausses' magnet adsorption deironing with magnetic force, after deironing, powder is mixed, again sieve, magnet adsorption deironing, make low-caffeine low content Tea Polyphenols 20kg, in product, content of caffeine is 0.1%, and polyphenol content is 50%.
Embodiment 3: a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its, it comprises the following steps:
S1. soak: fresh tea leaf in its 2000kg is placed in to digester, adds purified water 12000kg, constant temperature soaks 2h, and the mixed liquor in digester is crossed to 20 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 85 ℃;
S2. centrifugal: it is centrifugal 60s under 40 ℃, the pressure environment that is 0.3MPa that filtrate is placed in to temperature, discards precipitation, and centrifugate is for next-step operation; Wherein, the rotating speed of described centrifuge is 6800 turn/min;
S3. resin adsorption: centrifugate is splined on to HZ818 resin, and elution speed is 2m 3/ h, the caffeine in absorption filtrate, the efflux that collection solid content is 3%;
S4. film is concentrated: the efflux that the reverse osmosis membrane concentration step S3 that employing molecular cut off is 100 collects, and being concentrated into solid content is 40%;
S5. evaporation and concentration: concentrate is heated to 90 ℃, and evaporation and concentration to solid content is 42%, is cooled to normal temperature;
S6. spraying is dry: the concentrate that step S5 evaporation and concentration is crossed is sprayed dry, controls 80 ℃ of 200 ℃ of EATs, leaving air temps, the feed pressure 18MPa of spray dryer;
S7. deironing: dry spraying gained solid is pulverized with pulverizer, cross 60 mesh sieves, it is 12000 Gausses' magnet adsorption deironing with magnetic force, after deironing, powder is mixed, again sieve, magnet adsorption deironing, make low-caffeine low content Tea Polyphenols 23kg, in product, content of caffeine is 0.12%, and polyphenol content is 48%.
Embodiment 4: contrast test
1, from fresh tea passes, extract low-caffeine low content Tea Polyphenols:
S1. soak: fresh green tea 300g is placed in to digester, adds purified water 2100g, constant temperature soaks 2.2h, and the mixed liquor in digester is crossed to 20 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 90 ℃;
S2. centrifugal: it is centrifugal 65s under 45 ℃, the pressure environment that is 0.35MPa that filtrate is placed in to temperature, discards precipitation, and centrifugate is for next-step operation; Wherein, the rotating speed of described centrifuge is 6600 turn/min;
S3. resin adsorption: centrifugate is splined on to HZ818 resin, and elution speed is 2.2m 3/ h, the caffeine in absorption filtrate, the efflux that collection solid content is 2.8%;
S4. film is concentrated: the efflux that the reverse osmosis membrane concentration step S3 that employing molecular cut off is 100 collects, and being concentrated into solid content is 60%;
S5. evaporation and concentration: concentrate is heated to 95 ℃, and evaporation and concentration to solid content is 45%, is cooled to normal temperature;
S6. spraying is dry: the concentrate that step S5 evaporation and concentration is crossed is sprayed dry, controls 90 ℃ of 180 ℃ of EATs, leaving air temps, the feed pressure 18MPa of spray dryer;
S7. deironing: dry spraying gained solid being pulverized with pulverizer, crossed 80 mesh sieves, is 12000 Gausses' magnet adsorption deironing with magnetic force, after deironing, powder is mixed, sieves, magnet adsorption deironing again, makes low-caffeine low content Tea Polyphenols.
2, from stem tea, extract Tea Polyphenols:
Extracting method: S1. soaks: be 300g by dry green tea 150g(weight in wet base) be placed in digester, add purified water 2100g, constant temperature soaks 2.2h, and the mixed liquor in digester is crossed to 20 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 90 ℃;
All the other steps are with experiment 1.
3. detect: the weight of above-mentioned experiment 1,2 products obtained therefroms of accurate weighing, adopts following method to measure caffeine, the content of Tea Polyphenols and the yield of extract in product.
(1) assay method:
A. the content of caffeine adopts the analysis of HPLC method, and chromatographic condition is:
Chromatographic column: C184.6 × 150mm;
Mobile phase: water: methyl alcohol: phosphoric acid (77:23:0.1);
Flow velocity: 1.0ml/min;
Wavelength: 280nm;
Column temperature: 30 ℃;
A. the preparation of standard liquid: dry 24 hours above green tea control sample (through the standard items calibration of caffeine, EGCG one-component) 25mg of the phosphorus pentoxide of learning from else's experience, accurately weighed, put in 50ml volumetric flask, the about 40ml that adds water, ultrasonic processing is dissolved it completely, lets cool to room temperature, water is settled to scale, shaking up, is the filtering with microporous membrane of 0.45 μ m with aperture, to obtain final product.
B. need testing solution preparation: precision takes tea extract 25mg, puts 50ml(or 100ml) in volumetric flask, adding water ultrasonicly dissolves it in right amount, and taking-up lets cool, and adds water and is settled to scale, shake up, be the filtering with microporous membrane of 0.45 μ m with aperture, to obtain final product.
C. measure: accurate standard liquid and the each 20 μ l of need testing solution of drawing respectively, inject liquid chromatograph, measure, to obtain final product.
D. result is calculated
The content of each component calculates by following formula:
Each component (%)=(A sample× C contrast× V × Fi)/(A contrast× W) × 100%
In formula: W--sample weight, mg; A sample--sample peak area; A contrast--reference substance peak area; C contrast--reference substance concentration, mg/ml; V--test liquid volume, ml; Each component of Fi--is through the coefficient of discharge that contains of calibration.
B. the detection method of Tea Polyphenols:
A. reagent preparation:
Ferrous tartrate reagent: ferrous sulfate 1g and 5g sodium potassium tartrate tetrahydrate, water is settled to 1000ml after dissolving, and solution should keep in Dark Place.
Phosphate buffer:
Sodium hydrogen phosphate: take 23.377g sodium hydrogen phosphate, after water dissolves, constant volume is in 1000ml.
Potassium dihydrogen phosphate: take 9.078g potassium dihydrogen phosphate (baking 2 hours at 105 ℃) water and be settled to 1000ml after dissolving.
After getting respectively above-mentioned disodium phosphate soln 85ml and potassium dihydrogen phosphate 15ml and mixing, be pH7.5 phosphate buffer.
B. the preparation of test liquid and mensuration:
Standby for trial-production: accurately to weigh 100mg green-tea extract to 100ml volumetric flask, add 80ml purified water ultrasonic to dissolving completely, let cool to room temperature, add purified water constant volume, shake up, and the accurate 1ml solution of drawing is in 25ml volumetric flask, add 4ml water and 5ml ferrous tartrate solution, fully mix, then the phosphate buffer that adds pH7.5 is settled to scale, shake up, to obtain final product.
C. measure: measure with spectrophotometer (UV), make reference with blank, measure absorbance (A) at 540nm place.
D. result is calculated: the content of obtaining Tea Polyphenols by following formula.
Tea Polyphenols (%)=A × 2.88 × 100/m × 100%
In formula: m---example weight (mg); A----absorbance; 2.88----Tea Polyphenols absorption coefficient.
C. the calculating of recovery rate: yield (%)=product weight/tealeaves weight in wet base × 100% of extract
(2) experimental result: as shown in table 1:
Table 1: the contrast test of extracting low-caffeine low content Tea Polyphenols from stem tea and fresh tea passes
Figure BDA0000470063280000061
As known from Table 1: adopting fresh tea leaf in its to extract low-caffeine low content Tea Polyphenols products obtained therefrom weight is 33g, the yield of extract is 11%, be 30g and adopt stem tea to extract low-caffeine low content Tea Polyphenols products obtained therefrom weight, the yield of extract is 10%, all lower than adopting fresh tea leaf in its extraction method, content of caffeine is 0.34% to be significantly higher than fresh tea leaf in its extraction method, and adopting fresh tea leaf in its to extract products obtained therefrom polyphenol content is 47.6%, cured leaf extraction method products obtained therefrom polyphenol content difference is very little with adopting, illustrate that the method that adopts fresh leaf to extract low-caffeine low content Tea Polyphenols is better than adopting cured leaf extraction method.

Claims (4)

1. a method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its, is characterized in that, it comprises the following steps:
S1. soak: fresh tea leaf in its is placed in to digester, adds purified water constant temperature to soak 1.8~2.5h, the mixed liquor in digester is crossed to 18~24 mesh sieves, obtain filtrate; Wherein, described constant temperature soaking temperature is 65~100 ℃;
S2. centrifugal: it is centrifugal 50~70s under 30~50 ℃, the pressure environment that is 0.2~0.4MPa that filtrate is placed in to temperature, discards precipitation, and centrifugate is for next-step operation; Wherein, the rotating speed of described centrifuge is 6500~7000 turn/min;
S3. resin adsorption: centrifugate is splined on to HZ818 resin, the caffeine in absorption filtrate, the efflux that collection solid content is 2.5~3.5%;
S4. film is concentrated: the efflux that the reverse osmosis membrane concentration step S3 that employing molecular cut off is 100 collects, is concentrated into solid content >=20%;
S5. evaporation and concentration: concentrate is heated to temperature >=75 ℃, and evaporation and concentration to solid content is 40~50%, is cooled to normal temperature;
S6. spraying is dry: the concentrate that step S5 evaporation and concentration is crossed is sprayed dry, controls 75~100 ℃ of 160~220 ℃ of EATs, leaving air temps, the feed pressure 15~20MPa of spray dryer;
S7. deironing: dry spraying gained solid is pulverized with pulverizer, crossed 50~90 mesh sieves, use magnet adsorption deironing, after deironing, powder is mixed, again sieve, magnet adsorption deironing, make low-caffeine low content Tea Polyphenols.
2. a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its as claimed in claim 1, is characterized in that, the weight ratio of fresh tea leaf in its described in step S1 and purified water is 1:5~8.
3. a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its as claimed in claim 1, is characterized in that, elution speed described in step S3 is 1.8~2.4 m 3/ h.
4. a kind of method of extracting low-caffeine low content Tea Polyphenols from fresh tea leaf in its as claimed in claim 1, is characterized in that, the magnetic force of magnet described in step S7 is 10000~15000 Gausses.
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CN115553359A (en) * 2022-10-14 2023-01-03 成都华高生物制品有限公司 Preparation process of decaffeinated tea

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