CN102550993B - Method for preparing astringent persimmon powder with high micromolecule tannin content - Google Patents

Method for preparing astringent persimmon powder with high micromolecule tannin content Download PDF

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CN102550993B
CN102550993B CN201210043669XA CN201210043669A CN102550993B CN 102550993 B CN102550993 B CN 102550993B CN 201210043669X A CN201210043669X A CN 201210043669XA CN 201210043669 A CN201210043669 A CN 201210043669A CN 102550993 B CN102550993 B CN 102550993B
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juice
persimmon
ultrafiltration
tannin content
molecular weight
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CN102550993A (en
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李桂银
周治德
王仲民
操良丽
崔健
周怀营
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GUANGZHOU CIKANG BIOTECHNOLOGY Co.,Ltd.
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Guilin University of Electronic Technology
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  • Preparation Of Compounds By Using Micro-Organisms (AREA)
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  • Medicines Containing Plant Substances (AREA)
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Abstract

The invention discloses a method for preparing astringent persimmon powder with high micromolecule tannin content. The method comprises the following steps of: washing, smashing and juicing almost ripe persimmons, and performing enzymolysis, color protection, filtration, enzyme deactivation, sterilization and vacuum degassing, thus obtaining original persimmon juice; performing microfiltration on the original persimmon juice by use of a microfiltration film with the porosity of 0.22 mu m, performing primary ultrafiltration by use of an ultrafiltration film capable of retaining the molecular weight of 20,000, performing secondary ultrafiltration by use of an ultrafiltration film capable of retaining the molecular weight of 1,000, and collecting a filtrate obtained by the secondary ultrafiltration; and directly or further concentrating the filtrate, freezing and drying, thus obtaining the astringent persimmon powder with high micromolecule tannin content. Compared with the prior art, the method has the advantages that materials in all working procedures are at the temperature less than 60 DEG C, and most active substances in the persimmons are retained; and the astringent persimmon powder is high in quality and high in micromolecule tannin content, can be used as an anti-radiation, anti-oxidization and adsorption material, and is wide in application prospect.

Description

The preparation method of the puckery persimmon powder that a kind of little molecule tannin content is many
Technical field
The present invention relates to plant component extraction, the preparation method of the puckery persimmon powder that specifically a kind of little molecule tannin content is many.
Background technology
Astringent persimmon fruit has another name called Zhu fruit, is the very high fruit of a kind of nutritive value, enjoys the good reputation of " fruit Zisco product ", extensively plant in China, and be the important channel of increasing peasant income.Contain the puckery persimmon tannin in 2.0% left and right sides in the astringent persimmon fruit, also contain the necessary amino acid of carbohydrate, protein, human body, trace element, multivitamin, organic acid etc., have the human lymphocyte of inhibition leukaemia, hypotensive, remove the multiple efficacies such as interior free yl, absorption yttrium.Puckery persimmon tannin, higher with micromolecular tannin (molecular weight 1700) content in fresh Chinese olive, condensed tannin (molecular weight 10000-15000) content is lower.Persimmon fruit is in ripe, storage and process, and condensed tannin content has a larger increase and wherein little minute Chinese tannin descends obviously.Thereby the variation of tannin composition affects health care, absorption, the radioresistance effect of persimmon tannin.At present the research of persimmon is mainly concentrated on fresh-keeping, processing and acerbity removing method.Application for a patent for invention CN101328194 has announced a kind of persimmon powder and production technology thereof; It is after persimmon is squeezed the juice, and juice carries out enzymolysis, the enzyme that filters, goes out, concentrated, vacuum freeze drying and to make tannin content be 1%~99% powder, and the tannin content of this powder small molecular seldom, and is not strong to the metal biosorption effect.
Summary of the invention
Technical problem to be solved of the present invention provides the preparation method of the many puckery persimmon powders of a kind of little molecule tannin content.
The technical scheme that realizes the object of the invention is:
The preparation method of the puckery persimmon powder that a kind of little molecule tannin content is many comprises the steps:
1) select ripe very likely puckery persimmon, clean, broken, squeeze the juice the juice that obtains squeezing the juice;
2) juice of squeezing the juice is carried out complex enzyme hydrolysis: the juice of squeezing the juice is heated to 40-55 ℃ with sheath tube heater, in juice, add the pectase that activates good 0.005%-0.015% again, the apple amylase of 0.01%-0.025%, the papain enzyme of 0.008%-0.02%, stir, keep carrying out in 20-40 minute enzymolysis;
3) protect look: add the citric acid of 0.05%-0.15%, the phytic acid of 0.05%-0.15% is to step 2) juice protected look 20-40 minute;
4) filtration, sterilization, degassed: enzymolysis, the persimmon juice that protects behind the look are filtered; With the super high temperature instantaneous sterilizing machine enzyme and sterilizing that goes out, temperature is controlled at 121-125 ℃ with the persimmon juice after filtering; Carry out vacuum outgas after the sterilization, obtain persimmon fumet;
5) micro-filtration, ultrafiltration: persimmon fumet is selected the micro-filtration membrane of 0.22 μ m, carry out micro-filtration; The filtrate of crossing micro-filtration membrane is carried out ultrafiltration first time with the milipore filter of holding back 20000 molecular weight first, the filtrate of crossing behind the milipore filter is for the first time carried out ultrafiltration second time with the milipore filter of holding back 1000 molecular weight, the filtrate of the collection ultrafiltration second time again;
6) freeze drying: concentrate obtains persimmon powder through freeze drying, also the trapped fluid of the ultrafiltration second time directly can be obtained the many puckery persimmon powders of little molecule tannin content through freeze drying.
The present invention has following advantages and characteristic:
1, technology is new: compared with prior art, adopt complex enzyme zymohydrolysis, large molecule pectin, protein, starch in the persimmon are carried out enzymolysis, be convenient to tannin and effectively extract from persimmon, guarantee that simultaneously subsequent operation carries out smoothly.Adopt citric acid, phytic acid to protect look, the stability of the protection tannin tannin that particularly molecular weight is little.Adopt vacuum outgas, prevent the oxidation Decomposition of tanning matter.The milipore filter that 20000 molecular weight are held back in employing carries out the ultrafiltration first time, filtrate behind the mistake milipore filter first time is carried out the ultrafiltration second time with the milipore filter of holding back 1000 molecular weight again, collect the trapped fluid of for the second time ultrafiltration, guaranteed the content of the condensed tannin of molecular weight 10000-15000, guaranteed also that simultaneously molecular weight is the content of 1700 low-molecular-weight tannin.
2, all process steps material all is in below 60 ℃, has kept most of active material in the persimmon.
3, quality is good: the tannin content in this persimmon powder is high, as a kind of radioresistance, anti-oxidant and sorbing material, is with a wide range of applications.
The specific embodiment
The following stated embodiment understands the present invention in detail.In an embodiment, unless otherwise indicated, all umbers and percentage are all by mass.
Embodiment 1
Select ripe very likely puckery persimmon, clean, broken, squeeze the juice, the juice of squeezing the juice is heated to about 50 ℃ with sheath tube heater, squeeze into 3 tons of health storage tanks; Take by weighing 300g commodity pectase, the apple amylase of 360g, the papain enzyme of 300g activates enzyme, then joins in 3 tons of health storage tanks, stirs, and carries out enzymolysis; After keeping 30 minutes kinds, add the 300g citric acid, the phytic acid of 200ml protects look again; After 40 minutes kinds, the persimmon juice that enzymolysis is protected behind the look filters with plate and frame filter press; With super high temperature instantaneous sterilizing machine (UHT) enzyme and sterilizing that goes out, temperature is controlled at 121-125 ℃ with the persimmon juice after filtering, and the juice after the sterilization is squeezed into 3 tons of airtight storage tanks, and water flow vacuum pump carries out vacuum outgas, obtains persimmon fumet.With the micro-filtration membrane of persimmon fumet with 0.22 μ m, carry out micro-filtration operation, filter the impurity such as precipitation in the persimmon fumet, suspension, bacterium, rise and filter clarification; Then carry out ultrafiltration, the filtrate of crossing micro-filtration membrane is carried out the ultrafiltration first time with the milipore filter of holding back 20000 molecular weight first, the ultrafiltration later stage can add the pure water wash-out; Filtrate behind the mistake milipore filter first time is carried out the ultrafiltration second time with the milipore filter of holding back 1000 molecular weight again, and the ultrafiltration later stage can add the pure water wash-out; Collect the filtrate of for the second time ultrafiltration; With the filtrate sabot, thickness is 10mm, arrives quick-frozen under subzero 35 ℃ of conditions at subzero 28 ℃, all keeps more than the 4h after the crystallizations; Then under the 50-100Pa vacuum, under 65 ℃ of-85 ℃ of temperature about dry 16h, the persimmon material after drying finished unloads dish, beats powder, packing, just obtains persimmon powder.
Embodiment 2
Select ripe very likely puckery persimmon, clean, broken, squeeze the juice, the juice of squeezing the juice is heated to about 45 ℃ with sheath tube heater, squeeze into 3 tons of health storage tanks; Take by weighing the 240g pectase, the apple amylase of 360g, the papain enzyme of 360g activates enzyme, then joins in 3 tons of health storage tanks, stirs, and carries out enzymolysis; After keeping 35 minutes kinds, add the 200g citric acid, the phytic acid of 250ml protects look again; After protecting 20 minutes kinds of look, the persimmon juice that enzymolysis is protected behind the look filters with plate and frame filter press; With ultra high temperature short time sterilization (UHT) the machine enzyme and sterilizing that goes out, temperature is controlled at 121-125 ℃ with the persimmon juice after filtering, and the juice after the sterilization is squeezed into 3 tons of airtight storage tanks, and water flow vacuum pump carries out vacuum outgas, obtains persimmon fumet.With the micro-filtration membrane of persimmon fumet with 0.22 μ m, carry out micro-filtration operation, filter the impurity such as precipitation in the persimmon fumet, suspension, bacterium, rise and filter clarification; Then carry out ultrafiltration, the filtrate of crossing micro-filtration membrane is carried out the ultrafiltration first time with the milipore filter of holding back 20000 molecular weight first, the ultrafiltration later stage can add the pure water wash-out; Filtrate behind the mistake milipore filter first time is carried out the ultrafiltration second time with the milipore filter of holding back 1000 molecular weight again, and the ultrafiltration later stage can add the pure water wash-out; Collect the filtrate of for the second time ultrafiltration; Adopt centrifugal-film evaporator further concentrated filtrate, obtain the persimmon concentrate; With the sabot of persimmon concentrate, thickness is 10mm, arrives quick-frozen under subzero 35 ℃ of conditions at subzero 28 ℃, all keeps more than the 4h after the crystallizations; Then vacuum is at 50-80Pa, and temperature is controlled under 65 ℃-85 ℃ the condition, and about dry 16h, the persimmon material after drying finished unloads dish, beats powder, packing, just obtains persimmon powder.
Embodiment 3
Select ripe very likely puckery persimmon, clean, broken, squeeze the juice, the juice of squeezing the juice is heated to about 55 ℃ with sheath tube heater, squeeze into 5 tons of health storage tanks; Take by weighing the 7500g pectase, the apple amylase of 500g, the papain enzyme of 1000g activates enzyme, then joins in 5 tons of health storage tanks, stirs, and carries out enzymolysis; After keeping 40 minutes kinds, add the 1000g citric acid, the phytic acid of 500ml protects look again; After 20 minutes kinds, the persimmon juice that enzymolysis is protected behind the look filters with plate and frame filter press; With ultra high temperature short time sterilization (UHT) the machine enzyme and sterilizing that goes out, temperature is controlled at 121-125 ℃ with the persimmon juice after filtering, and the juice after the sterilization is squeezed into 5 tons of airtight storage tanks, and water flow vacuum pump carries out vacuum outgas, obtains persimmon fumet.With the micro-filtration membrane of persimmon fumet with 0.22 μ m, carry out micro-filtration operation, filter the impurity such as precipitation in the persimmon fumet, suspension, bacterium, rise and filter clarification; Then carry out ultrafiltration, the filtrate of crossing micro-filtration membrane is carried out the ultrafiltration first time with the milipore filter of holding back 20000 molecular weight first; Filtrate behind the mistake milipore filter first time is carried out the ultrafiltration second time with the milipore filter of holding back 1000 molecular weight again, and the ultrafiltration later stage can add the pure water wash-out; Collect the filtrate of for the second time ultrafiltration; With the filtrate sabot, thickness is 10mm, arrives quick-frozen under subzero 35 ℃ of conditions at subzero 28 ℃, all keeps more than the 4h after the crystallizations; Then under the 50-100Pa vacuum, under 65 ℃ of-85 ℃ of temperature about dry 16h, the persimmon material after drying finished unloads dish, beats powder, packing, just obtains persimmon powder.

Claims (2)

1. the preparation method of one kind little molecule tannin content puckery persimmon powder how is characterized in that: comprise the steps:
1) select ripe very likely puckery persimmon, clean, broken, squeeze the juice the juice that obtains squeezing the juice;
2) juice of squeezing the juice is carried out enzymolysis: the juice of squeezing the juice is heated to 40-55 ℃ with sheath tube heater, in juice, add the pectase that activates good 0.005%-0.015% again, the apple amylase of 0.01%-0.025%, the papain of 0.008%-0.02%, stir, keep carrying out in 20-40 minute enzymolysis;
3) protect look: add the citric acid of 0.05%-0.15%, the phytic acid of 0.05%-0.15% is to step 2) juice protected look 20-40 minute;
4) filtration, sterilization, degassed: enzymolysis, the persimmon juice that protects behind the look are filtered; With the super high temperature instantaneous sterilizing machine enzyme and sterilizing that goes out, temperature is controlled at 121-125 ℃ with the persimmon juice after filtering; Carry out vacuum outgas after the sterilization, obtain persimmon fumet;
5) micro-filtration, ultrafiltration: persimmon fumet is selected the micro-filtration membrane of 0.22 μ m, carry out micro-filtration; The filtrate of crossing micro-filtration membrane is carried out ultrafiltration first time with the milipore filter of holding back 20000 molecular weight first, use again the milipore filter of holding back 1000 molecular weight to carry out the ultrafiltration second time filtrate of crossing behind the milipore filter for the first time;
6) collect the trapped fluid of for the second time ultrafiltration, trapped fluid is directly or further concentrated after, again through freeze drying, namely obtain molecular weight and be 1700 the many puckery persimmon powders of persimmon tannin content.
2. the many puckery persimmon powders of little molecule tannin content that prepare with the described preparation method of claim 1.
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CN102908275A (en) * 2012-11-05 2013-02-06 桂林电子科技大学 Method for controlling moisture absorption and color change of persimmon powder
CN103340368A (en) * 2013-07-19 2013-10-09 广西壮族自治区中国科学院广西植物研究所 Preparation method of astringent-persimmon dry powder containing persimmon-slag tannin
CN103719765B (en) * 2013-12-31 2015-08-05 李卉 A kind of Tuo Se Fei sheet and preparation method thereof
CN104478950B (en) * 2014-12-19 2017-04-05 桂林得坤生物科技股份有限公司 A kind of method of the persimmon tannin from Fructus Kaki more than extraction small molecule tannin content
CN104447897B (en) * 2014-12-19 2017-06-06 桂林得坤生物科技股份有限公司 A kind of method that persimmon tannin is extracted from persimmon
CN104788511B (en) * 2015-03-31 2017-10-31 桂林得坤生物科技股份有限公司 A kind of method of persimmon tannin from persimmon more than preparation small molecule tannin content
CN105581217B (en) * 2015-12-14 2018-02-13 山东省果树研究所 A kind of method of arsenic in removal cider

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CN1040616C (en) * 1993-09-16 1998-11-11 孙印全 Puckery removed persimmon juice and its instant powder for beverage and producing process thereof
CN101215498B (en) * 2007-12-28 2011-05-11 仲恺农业技术学院 Method for producing acerbity-removing persimmon wine
CN101328194A (en) * 2008-07-22 2008-12-24 恭城汇坤农品有限公司 Persimmon powder and production process thereof

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Application publication date: 20120711

Assignee: GUANGZHOU CANYON BIOTECHNOLOGY CO.,LTD

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Denomination of invention: Method for preparing astringent persimmon powder with high micromolecule tannin content

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Address before: Huadu District, Guangdong city of Guangzhou province Xinya street 510800 village two team wide blue Ke Industrial Park Building No. 1

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