CN102174611A - Process for degreasing low methoxyl pectin - Google Patents
Process for degreasing low methoxyl pectin Download PDFInfo
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- CN102174611A CN102174611A CN2010106061034A CN201010606103A CN102174611A CN 102174611 A CN102174611 A CN 102174611A CN 2010106061034 A CN2010106061034 A CN 2010106061034A CN 201010606103 A CN201010606103 A CN 201010606103A CN 102174611 A CN102174611 A CN 102174611A
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Abstract
The invention relates to a process for degreasing low methoxyl pectin. The process comprises the following steps of: a, pomace cleaning; b, pectin extraction and pigment removal; c, pectin methylesterase catalyzed hydrolysis: regulating the pH value of the prepared high methoxyl pectin concentrate to be between 3.0 and 4.5, adding pectin methylesterase in an amount which is 0.05 percent of the weight of the pectin concentrate, and preserving the heat at the temperature of between 30 and 45 DEG C; d, ethanol sedimentation; and e, finished product formation. The process for degreasing the low methoxyl pectin has low requirement for the raw materials for producing the pectin, destroys the pectin molecular chain in the degreasing process, and keeps the activity of the pectase.
Description
Technical field
The present invention relates to a kind of method, what be specifically related to a kind of pectin takes off ester technology, and what the present invention related more specifically to a kind of low-methoxy pectin takes off ester technology.
Technical background
The ester method of taking off of pectin has 3 kinds usually: acid system, enzyme process and alkaline process take off ester, and 3 kinds of methods respectively have relative merits.It is higher that acid system takes off ester pectin polygalacturonic acid content, but speed of response is slow, and with under the concentration conditions, it takes off ester speed and takes off 0.01% of ester less than alkaline process in equality of temperature, and elevated temperature can fast reaction speed, but the depolymerization of pectin chain is accelerated greatly simultaneously; It is easy that enzyme process takes off ester technology, but gained pectin is lower than additive method owing to the nonrandom distribution of methoxyl group in the molecule causes gel strength; It is fast that alkaline process commonly used takes off ester speed in the production, but pectin is when alkaline process takes off ester, methoxy content reduces in molecule, and the depolymerization that also can produce pectin molecule simultaneously, promptly so-called β-elimination reaction.Following chemical equation:
β-elimination reaction can cause pectin molecule amount, viscosity and gelling ability to descend, the de-ester reaction of pectin and β-elimination reaction often take place simultaneously, just reaction conditions is not simultaneously, both speed of response differences, it is exactly that they belong to competitive reaction that these 2 kinds of chemical reactions also have characteristics: the former makes, and methoxy content reduces in the pectin, and the latter must just can carry out under the condition that methoxyl group exists, both methoxyl groups of vying each other, de-ester reaction has arrived certain phase, because the minimizing of methoxy content, 2 kinds of chemical reaction velocities all can reduce.
In sum, the ester technology of taking off of traditional mode of production low-methoxy pectin is in the process that pectin extracts, and adds polygalacturonase and directly takes off ester.This technology mainly contains following shortcoming:
The first, in leaching process, directly add polygalacturonase, to producing the raw material of pectin, specification of quality is than higher, and the raw material that some gel contents are low is in leaching process, because polygalacturonase acts on for a long time, causes a large amount of pectin to go to pot, make finally can't extract pectin.
The second, directly take off ester at leaching process, because that pectin extracts the required time is long, the pectin molecule chain that caused the polygalacturonase considerable damage has reduced pectin grade and gamma value, has had a strong impact on the pectin quality.
Three, at leaching process, use polygalacturonase to take off ester owing to need higher temperature in the leaching process, thus havoc the activity of polygalacturonase, make a large amount of polygalacturonases not play corresponding effect, thereby cause the polygalacturonase consumption excessive.
Summary of the invention
The purpose of this invention is to provide a kind of low to the ingredient requirement of producing pectin, in taking off the ester process, destroy the pectin molecule chain less, keep polygalacturonase active low-methoxy pectin take off ester technology.
Theoretical foundation of the present invention is: 1, concentration of pectin is to taking off the influence of ester: for reducing production costs, the ester that falls of high ester pectin adopts concentrated solution to carry out.Concentrated solution concentration is too high then mobile bad, influences the operation of back operation; If concentrated solution concentration is too low, though increased the flowability of liquid, the alcohol consumption that has used when having increased precipitating can increase production cost equally.2, pH value in reaction is to taking off the influence of ester: pH value in reaction is high more, and its finished product gamma value is low more; Otherwise pH value in reaction is low more, and its finished product gamma value is high more.PH value in reaction is high more, and its finished product degree of gelation is low more; Otherwise pH value in reaction is low more, and its finished product degree of gelation is high more.3, the reaction times is to the influence of degreasing: the reaction times is long more, and its finished product gamma value is low more; Otherwise the reaction times is short more, and its finished product gamma value is high more.4, temperature of reaction is to taking off the influence of ester: temperature of reaction is high more, and its finished product gamma value is low more; Otherwise temperature of reaction is low more, and its finished product gamma value is high more.Temperature of reaction is high more, and its finished product degree of gelation is low more; Otherwise temperature of reaction is low more, and its finished product degree of gelation is high more.
Technical scheme of the present invention is, a kind of low-methoxy pectin take off ester technology, it comprises following processing step:
A. pomace is cleaned: will be crushed to 60 purpose oranges and tangerines pomaces and 70 ℃ of water mix by 1: 20 weight ratio, and stir and soak 50min, be 70～80% with the pomace after cleaning with pressing that the band machine squeezes to containing moisture weight;
B. pectin extracts and removes pigment: the pomace after will cleaning mixes according to 1: 30 weight ratio with water, adds acid for adjusting pH value 2.0～2.9,70～90 ℃ of insulation 1.5～5h, and the resin that adds pomace weight 20%-50% weight simultaneously extracts.After the end to be extracted, separation and Extraction liquid and residue also filter clarification by leaf worry machine, doubly concentrate ratio according to 2-4 then, carry out vacuum concentration.
C. pectinesterase enzymatic hydrolysis: will make high methoxyl pectin concentrated solution pH value and be adjusted to 3.0～4.5, and add 0.5 ‰ pectin methylesterases of fructose concentrating liquid weight, 30～45 ℃ of insulations;
D. ethanol sedimentation: pectin solution pH value is transferred to 3.8～5.0, will be preheated to the weight ratio mixed precipitation of 30～50 ℃ 50～60% ethanol and pectin solution by 4: 1;
E. finished product is made: with sedimentation pectin through centrifugal, squeezing, dry finished product.
Technique effect of the present invention is:
The low-methoxy pectin production technique that the present invention breaks traditions is (in extracting the pectin process, directly take off ester and produce low-ester pectin), innovate a kind of novel low-methoxy pectin production technique promptly on the basis of the concentrated solution of producing high ester pectin, adopted Rohapect MPE to take off ester technology again.The first, Rohapect MPE directly acts on concentrated pectin solution, has significantly reduced the consumption of Rohapect MPE; The second, Rohapect MPE directly acts on concentrated pectin solution, and we can control the temperature of fructose concentrating liquid, keeps the activity of Rohapect MPE, gives full play to the ester effect of taking off of Rohapect MPE.The 3rd, because Rohapect MPE directly acts on pure fructose concentrating liquid, after finishing esterase and taking off ester, can promptly enter the precipitation link, improved production efficiency greatly, reduced the production cost of low-methoxy pectin.
Embodiment:
In order to understand better and to implement, take off ester technology below in conjunction with a kind of low-methoxy pectin of example in detail the present invention.
Embodiment 1, will be crushed to 60 order apple pomaces and 70 ℃ of water carry out soaking and stirring 50min with 1: 20 weight ratio, removes partial pigment, the pomace after cleaning pressed the band machine squeeze to water content 75%; Mix by 1: 20 weight ratio with water then, add acid for adjusting pH value to 2.0,70 ℃ of insulation 1.5h, after the end to be extracted, separation and Extraction liquid and residue also filter clarification by leaf worry machine, according to 2 times of concentrated ratios, carry out vacuum concentration then.To make high methoxyl pectin concentrated solution pH value and be adjusted to 3.0, and add 0.5 ‰ pectin methylesterases of fructose concentrating liquid weight, 30 ℃ of insulations are determined soaking time according to the gamma value of product requirement.After waiting to take off ester and finishing, pectin solution pH value is transferred to 4.0,50% alcohol that is preheated to 30 ℃ is mixed stirring with pectin solution with 4: 1 weight ratio precipitate, with precipitation carry out centrifugal, squeezing, drying makes the low-methoxy pectin finished product.Products obtained therefrom and QB2484-2000 China National Light Industrial Products Department standard compare: as following table
According to last table as can be known, the low-methoxy pectin that adopts example 1 method to produce, the requirement of the equal accord with Q B2484-2000 of its physical and chemical index, and the degree of gelation of products obtained therefrom and pectin purity galacturonic acid are all than higher, therefore we can say the low-methoxy pectin that this method is produced, best in quality.
Embodiment 2, will be crushed to 60 order apple pomaces and 70 ℃ of water carry out soaking and stirring 50min with 1: 20 weight ratio, remove partial pigment, the pomace after cleaning is pressed the band machine squeeze to water content 75%; Mix by 1: 20 weight ratio with water then, add acid for adjusting pH value to 2.4,80 ℃ of insulation 2.5h, after the end to be extracted, separation and Extraction liquid and residue also filter clarification by leaf worry machine, according to 2.4 times of concentrated ratios, carry out vacuum concentration then.To make high methoxyl pectin concentrated solution pH value and be adjusted to 3.9, and add 0.5 ‰ pectin methylesterases of fructose concentrating liquid weight, 40 ℃ of insulations are determined soaking time according to the gamma value of product requirement.After waiting to take off ester and finishing, pectin solution pH value is transferred to 4.2,50% alcohol that is preheated to 40 ℃ is mixed stirring with pectin solution with 4: 1 weight ratio precipitate, with precipitation carry out centrifugal, squeezing, drying makes the low-methoxy pectin finished product.Products obtained therefrom and QB2484-2000 China National Light Industrial Products Department standard compare: as following table
According to last table as can be known, the low-methoxy pectin that adopts example 2 methods to produce, the requirement of the equal accord with Q B2484-2000 of its physical and chemical index, and the degree of gelation of products obtained therefrom and galacturonic acid number are all than higher, therefore we can say the low-methoxy pectin that this method is produced, best in quality.
Embodiment 3, will be crushed to 60 order apple pomaces and 70 ℃ of water carry out soaking and stirring 50min with 1: 20 weight ratio, remove partial pigment, the pomace after cleaning is pressed the band machine squeeze to water content 75%; Mix by 1: 20 weight ratio with water then, add acid for adjusting pH value to 2.9,90 ℃ of insulation 5h, after the end to be extracted, separation and Extraction liquid and residue also filter clarification by leaf worry machine, according to 4 times of concentrated ratios, carry out vacuum concentration then.To make high methoxyl pectin concentrated solution pH value and be adjusted to 5.0, and add 0.5 ‰ pectin methylesterases of fructose concentrating liquid weight, 50 ℃ of insulations are determined soaking time according to the gamma value of product requirement.After waiting to take off ester and finishing, pectin solution pH value is transferred to 5.0,50% alcohol that is preheated to 50 ℃ is mixed stirring with pectin solution with 4: 1 weight ratio precipitate, with precipitation carry out centrifugal, squeezing, drying makes the low-methoxy pectin finished product.Products obtained therefrom and QB2484-2000 China National Light Industrial Products Department standard compare: as following table
According to last table as can be known, the low-methoxy pectin that adopts example 2 methods to produce, the requirement of the equal accord with Q B2484-2000 of its physical and chemical index, and the degree of gelation of products obtained therefrom and galacturonic acid number are all than higher, therefore we can say the low-methoxy pectin that this method is produced, best in quality.
Claims (1)
- A low-methoxy pectin take off ester technology, it comprises following processing step:A. pomace is cleaned: will be crushed to 60 purpose oranges and tangerines pomaces and 70 ℃ of water mix by 1: 20 weight ratio, and stir and soak 50min, be 70～80% with the pomace after cleaning with pressing that the band machine squeezes to containing moisture weight;B. pectin extracts and removes pigment: the pomace after will cleaning mixes according to 1: 30 weight ratio with water, adds acid for adjusting pH value 2.0～2.9,70～90 ℃ of insulation 1.5～5h, and the resin that adds pomace weight 20%-50% weight simultaneously extracts.After the end to be extracted, separation and Extraction liquid and residue also filter clarification by leaf worry machine, doubly concentrate ratio according to 2-4 then, carry out vacuum concentration.C. pectinesterase enzymatic hydrolysis: will make high methoxyl pectin concentrated solution pH value and be adjusted to 3.0～4.5, and add 0.5 ‰ pectin methylesterases of fructose concentrating liquid weight, 30～45 ℃ of insulations;D. ethanol sedimentation: pectin solution pH value is transferred to 3.8～5.0, will be preheated to the weight ratio mixed precipitation of 30～50 ℃ 50～60% ethanol and pectin solution by 4: 1;E. finished product is made: with sedimentation pectin through centrifugal, squeezing, dry finished product.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059165A (en) * | 2014-06-23 | 2014-09-24 | 中国农业大学 | Low ester pectin and preparation method thereof |
| CN104379002A (en) * | 2012-07-02 | 2015-02-25 | 荷兰联合利华有限公司 | Concentrate food composition in the form of a gel |
| CN104975055A (en) * | 2015-07-01 | 2015-10-14 | 安徽亿源生物工程有限公司 | Degreasing method for low-ester pectin |
| CN105400847A (en) * | 2015-10-14 | 2016-03-16 | 烟台安德利果胶股份有限公司 | High-methoxyl pectin with high protein stability and preparation method thereof |
| CN111920032A (en) * | 2020-08-19 | 2020-11-13 | 烟台安德利果胶股份有限公司 | Preparation method of modified pectin with high emulsibility and low viscosity, modified pectin with high emulsibility and low viscosity and application of modified pectin |
| CN112266941A (en) * | 2020-09-30 | 2021-01-26 | 浙江果源康品生物科技有限公司 | Method for producing micromolecular pectin by combining enzyme and alkali |
| CN114634655A (en) * | 2022-03-24 | 2022-06-17 | 重庆檬泰生物科技有限公司 | Pectin production process for coating probiotics |
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| CN1041865A (en) * | 1988-10-10 | 1990-05-09 | 烟台大学 | Produce pectin jelly technology with apple waste |
| CN1310186A (en) * | 2001-01-19 | 2001-08-29 | 华北工学院 | pectin producing method |
| CN101073384A (en) * | 2006-05-17 | 2007-11-21 | 烟台安德利果胶有限公司 | Production of low-methoxy apple pectin |
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Patent Citations (3)
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| CN1041865A (en) * | 1988-10-10 | 1990-05-09 | 烟台大学 | Produce pectin jelly technology with apple waste |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104379002A (en) * | 2012-07-02 | 2015-02-25 | 荷兰联合利华有限公司 | Concentrate food composition in the form of a gel |
| CN104379002B (en) * | 2012-07-02 | 2017-06-09 | 荷兰联合利华有限公司 | Emergenoy ration composition of gel form |
| CN104059165A (en) * | 2014-06-23 | 2014-09-24 | 中国农业大学 | Low ester pectin and preparation method thereof |
| CN104975055A (en) * | 2015-07-01 | 2015-10-14 | 安徽亿源生物工程有限公司 | Degreasing method for low-ester pectin |
| CN105400847A (en) * | 2015-10-14 | 2016-03-16 | 烟台安德利果胶股份有限公司 | High-methoxyl pectin with high protein stability and preparation method thereof |
| CN105400847B (en) * | 2015-10-14 | 2018-10-02 | 烟台安德利果胶股份有限公司 | A kind of high-ester pectin and preparation method thereof of high protein stability |
| CN111920032A (en) * | 2020-08-19 | 2020-11-13 | 烟台安德利果胶股份有限公司 | Preparation method of modified pectin with high emulsibility and low viscosity, modified pectin with high emulsibility and low viscosity and application of modified pectin |
| CN112266941A (en) * | 2020-09-30 | 2021-01-26 | 浙江果源康品生物科技有限公司 | Method for producing micromolecular pectin by combining enzyme and alkali |
| CN114634655A (en) * | 2022-03-24 | 2022-06-17 | 重庆檬泰生物科技有限公司 | Pectin production process for coating probiotics |
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Application publication date: 20110907 |