CN103739741B - A kind of method extracting pectin from fermentation haw thorn wine pomace - Google Patents

A kind of method extracting pectin from fermentation haw thorn wine pomace Download PDF

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CN103739741B
CN103739741B CN201310712689.6A CN201310712689A CN103739741B CN 103739741 B CN103739741 B CN 103739741B CN 201310712689 A CN201310712689 A CN 201310712689A CN 103739741 B CN103739741 B CN 103739741B
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pectin
water
alcohol
pomace
hawthorn
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CN103739741A (en
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杜金华
赵志云
张斌
金玉红
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Shandong Agricultural University
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Shandong Agricultural University
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Abstract

The invention provides a kind of method extracting pectin from fermentation haw thorn wine pomace, material-water ratio 1 ~ the 2:2 of fermentation haw thorn pomace and water will be distilled, distillation residue are lixiviate 1h at 85 ~ 95 DEG C, 1% ~ 5%(m/v) wash decolouring 30 ~ 90min at granulated active carbon 80 DEG C, low temperature alcohol precipitation (5 DEG C; 55%(V/V) alcohol; 12h), room temperature alcohol wash (70%(V/V) alcohol; 1h); Protopectin-in slag is hydrolyzed to water soluble pectin further and transfers in water, press filtration obtains filtrate.Filtrate and vinasse are merged, centrifugal, obtain the pectin solution of clear.With granulated activated carbon decoloring, alcohol precipitation that deionized water is washed, after drying, pulverizing, obtain hawthorn pectin dry powder.The present invention compares acid solution hydrolysis method, need not acid adding in addition in pectin extraction process, avoids and introduce new acidic substance in system, reduces difficulty for residue after extracting pectin develops.

Description

A kind of method extracting pectin from fermentation haw thorn wine pomace
(1) art
The present invention relates to a kind of method extracting pectin from fermentation haw thorn wine pomace, object is the utilization ratio improving food resource, belongs to food processing technology field.
(2) background technology
Hawthorn, has another name called Fruit of Pashi Pear, haw, kermes fruit, has very high nutrition and medical value.Hawthorn is containing multivitamin, Crategolic acid, tartrate, citric acid, oxysuccinic acid etc., also containing the mineral substance such as flavonoid, lactone, carbohydrate, protein, fat and calcium, phosphorus, iron, contained lipolytic enzyme can promote the digestion of fat food, promotes gastric secretion and increases the functions such as stomach endoenzyme element.The traditional Chinese medical science is thought, hawthorn has that long-pendingization that disappear is stagnant, convergence only dysentery, the effect such as activate blood circulation and disperse blood clots, and cures mainly the diseases such as eating accumulation, chest diaphragm spleen are full, the amenorrhoea of hernia blood stasis.Containing the pharmaceutical cpd such as mountain terpene and flavonoid in hawthorn, there is significant vasodilation and hypotensive effect, have the function strengthening cardiac muscle, arrhythmia, adjusting blood lipid and cholesterol level.Flavonoid contained by hawthorn and the substance such as vitamins C, carotene block and reduce the generation of free radical, and the immunizing power of energy enhancing body, has anti-aging, anticancer effect.In hawthorn, pectin has radiation protection, can take away radioelement (strontium, cobalt, palladium etc.) in body, has absorption and antibacterial properties, can remove intestinal bacteria, toxin hold onto moisture, therefore can treat abdominal pain diarrhea.
Pectin is a kind of acidic polysaccharose material in plant, and it is generally white to pale yellow powder, is slightly with tart flavour, have water-soluble, industrial namely separable, its molecular weight about 50,000 ~ 300,000, mainly being present in cell walls and the cell internal layer of plant, is the support substance of inner cell.Jelling agent made by food, thickening material, stablizer, suspension agent, emulsifying agent, flavouring synergistic agent, and can be used for makeup, to protection skin, prevent ultraviolet radiation, wound is treated in smelting, and beautifying face and moistering lotion all deposits certain effect.Pectin can be divided into high methoxyl pectin and low-methoxy pectin by molecular structure, there is the mainly high methoxyl pectin in Fructus Crataegi, its water-swelling, is dissolved in water and becomes thickness, and special composition decides the distinctive processing characteristics of hawthorn and distinctive converted products.
In hawthorn, pectin content occupies first of fruit, reaches 6.4%, and after fermentation, residual more pectin in Hawthorn Fruit Wine pomace (after brewageing Hawthorn Fruit Wine remaining pomace), have impact on the further processing and utilization of hawthorn pomace.China's hawthorn output is large, about 1,000,000 tons, and the emphasis studied for a long time all concentrates on and utilizes hawthorn as edible, processed can, fruit juice and fruit wine, and a large amount of pomace goes out of use, and causes the waste of resource and the pollution of environment.Therefore, how effectively from fermentation haw thorn wine pomace, extracting pectin, and maximally improve the quality of pectin, will be the important means that enterprise is cost-saving, increase the benefit, and be the current a great problem faced.
(3) summary of the invention
In order to solve the problem, the invention provides a kind of method extracting pectin from fermentation haw thorn wine pomace.Hawthorn pomace tissue looseness after zymamsis, the materials such as sugar wherein, pigment have been fully extracted out, and starch has been decomposed utilization, and pectin obtains Partial digestion during the fermentation, still containing part organic acid in slag.Compared with traditional pectin preparation technology, fermentation haw thorn pomace of the present invention does not need to wash the soluble components such as sugar, pigment except residual in removing slag, and does not need to add the starch (because of without starch) in amylase degrades slag, does not need other acid adding in pectin extraction process.The distillation that added water by fermentation haw thorn wine pomace obtains hawthorn liquor, and the part pectin in slag dissolves and enters in vinasse in still-process.Be separated distillation residue and raffinate.Add the deionized water of equivalent in distillation residue, be heated to 85 ~ 95 DEG C of lixiviate 1h.Protopectin-in slag is hydrolyzed to water soluble pectin further and transfers in water, press filtration obtains filtrate.Filtrate and vinasse are merged, centrifugal, obtain the pectin solution of clear.With granulated activated carbon decoloring, alcohol precipitation that deionized water is washed, after drying, pulverizing, obtain hawthorn pectin dry powder.
From fermentation haw thorn wine pomace, extract a method for pectin, comprise the steps:
Hawthorn Fruit Wine pomace after fermentation wraps, according to pomace and water 1 ~ 2:2(m/m by 1) ratio add deionized water, distill out hawthorn alcohol, filtering separation distillation residue and raffinate.
2 according to distillation residue and water 1:1(m/m) ratio, in distillation residue, add deionized water, collecting by filtration filtrate after 85 ~ 95 DEG C of stirring and leaching 1h.
3 by step 1) gained vinasse and step 2) filtrate of collecting mixing, 4500r/min is centrifugal, and 10min obtains supernatant liquor.
4 add washing granulated active carbon in supernatant liquor, and to supernatant liquor, contain washing granulated active carbon concentration is 1% ~ 5%(m/v); Reheat to 60 ~ 80 DEG C of decolouring 30 ~ 90min; Filtering separation gac, obtains the colourless permeate of clear;
5 filtrates obtain concentrated solution in the half that 80 DEG C are concentrated into original volume;
6 in concentrated solution, add concentration be 65%(V/V) edible ethanol makes alcohol concn in mixed system reach 55%(V/V) more than, place 12h for 5 DEG C and carry out alcohol precipitation, press filtration obtains filter residue.Adding concentration in filter residue is 95%(V/V) edible ethanol makes alcohol concn in mixed system reach 70%(V/V), stir 1h with the impurity in abundant stripping pectin, press filtration must be wet pectin.
7 wet pectin in 50 ~ 60 DEG C of oven dry, pulverize to obtain dry fruit glue.
The invention has the beneficial effects as follows:
The present invention utilizes Hawthorn Fruit Wine pomace after zymamsis to extract pectin first, and the materials such as the sugar in slag, starch, pigment have been fully extracted or starch utilizes, and saves rinsing except sugar, depigmentation, process except starch; Hawthorn quality after fermentation is loosened, and is beneficial to the extraction of pectin; Solve the problem of the waste of fermentation haw thorn wine pomace, contaminate environment, achieve making full use of of haw raw material.The pectin of the present invention first while distillation fermentation haw thorn pomace extracts hawthorn alcohol (preparation hawthorn liquor) in extractive distillation raffinate, turns waste into wealth, reduces three-protection design cost, save in pectin extraction process enzyme step of going out.The present invention compares acid solution hydrolysis method, need not acid adding in addition in pectin extraction process, avoids and introduce new acidic substance in system, reduces difficulty for residue after extracting pectin develops.
The present invention determines each processing parameter in leaching process, distillation fermentation haw thorn pomace and the material-water ratio 1 ~ 2:2 of water, and distillation residue are lixiviate 1h at 85 ~ 95 DEG C, 1% ~ 5%(m/v) wash decolouring 30 ~ 90min at granulated active carbon 80 DEG C, low temperature alcohol precipitation (5 DEG C; 55%(V/V) alcohol; 12h), room temperature alcohol wash (70%(V/V) alcohol; 1h).
Pectin of the present invention wets pectin color for white, and dry fruit glue color is faint yellow, galacturonic acid content more than 65%.
(4) accompanying drawing explanation
Fig. 1 extracts the schema of pectin from fermentation haw thorn wine pomace
(5) embodiment
Embodiment 1
1 distillation afterwards Hawthorn Fruit Wine pomace (pectin content the is weight in wet base 1.2%) gauze that will ferment wraps up, according to pomace and water 1:2(m/m) ratio add deionized water and distill out hawthorn alcohol (the hawthorn alcohol distilled out may be used for making hawthorn liquor).Be separated distillation residue and raffinate.
2 extract according to slag water ratio 1:1(m/m) ratio, add deionized water in distillation residue, 85 ~ 95 DEG C of stirring and leaching 1h.
Press filtration after 3 press filtration lixiviates, a small amount of hot water injection's filter residue, collects filtrate.
4 centrifugal mixing filtrate and vinasses, 4500r/min is centrifugal, and 10min obtains supernatant liquor.
Containing washing granulated active carbon concentration in interpolation washing granulated active carbon to supernatant liquor in 5 decolouring centrifuged supernatant is 2%(m/v), be heated to 70 DEG C of decolouring 90min.
6 filter filter pulp filtering separation gac, obtain clear filtrate.
7 concentrated filtrates are concentrated into the half of original volume in 80 DEG C.
It is 65%(V/V that 8 alcohol precipitations add concentration in concentrated solution) edible ethanol makes alcohol concn in mixed system reach 55%(V/V), place 12h for 5 DEG C.
After 9 press filtration alcohol precipitations, solution press filtration must be wet pectin.
10 dry wet pectin in 50 ~ 60 DEG C of oven dry, pulverize to obtain dry fruit glue.
Wet pectin color clear obtained as stated above, color slightly black after dry, wherein galacturonic acid content reaches 40.5%.
Embodiment 2
1 distillation afterwards Hawthorn Fruit Wine pomace (pectin content the is weight in wet base 1.2%) gauze that will ferment wraps up, according to pomace and water 1:2(m/m) ratio add deionized water, distill out hawthorn alcohol.Be separated distillation residue and raffinate.
2 extract according to slag water ratio 1:1(m/m) ratio, add deionized water in distillation residue, 85 ~ 95 DEG C of stirring and leaching 1h.
Press filtration after 3 press filtration lixiviates, a small amount of hot water injection's filter residue, collects filtrate.
4 centrifugal mixing filtrate and vinasses, 4500r/min is centrifugal, and 10min obtains supernatant liquor.
Containing washing granulated active carbon concentration in interpolation washing granulated active carbon to supernatant liquor in 5 decolouring centrifuged supernatant is 2%; Heating of supernatant to 80 DEG C decolouring 30min.
6 filter filter pulp filtering separation gac, obtain clear filtrate.
7 concentrated filtrates are concentrated into the half of original volume in 80 DEG C.
It is 65%(V/V that 8 alcohol precipitations add concentration in concentrated solution) edible ethanol makes alcohol concn in mixed system reach 55%(V/V), place 12h for 5 DEG C.
After 9 press filtration alcohol precipitations, solution press filtration must be wet pectin.
10 dry wet pectin in 50 ~ 60 DEG C of oven dry, pulverize to obtain dry fruit glue.
Wet pectin color clear obtained as stated above, after dry, color is slightly rubescent, and wherein galacturonic acid content reaches 62.3%.
Embodiment 3
1 distillation afterwards Hawthorn Fruit Wine pomace (pectin content the is weight in wet base 1.2%) gauze that will ferment wraps up, according to pomace and water 1:2(m/m) ratio add deionized water, distill out hawthorn alcohol.Be separated distillation residue and raffinate.
2 extract according to slag water ratio 1:1(m/m) ratio, add deionized water in distillation residue, 85 ~ 95 DEG C of stirring and leaching 1h.
Press filtration after 3 press filtration lixiviates, a small amount of hot water injection's filter residue, collects filtrate.
4 centrifugal mixing filtrate and vinasses, 4500r/min is centrifugal, and 10min obtains supernatant liquor.
Add in 5 decolouring centrifuged supernatant in washing granulated active carbon to supernatant liquor containing washing granulated active carbon concentration 2%(m/v), heating of supernatant to 80 DEG C decolouring 30min.
6 filter filter pulp filtering separation gac, obtain clear filtrate.
7 concentrated filtrates are concentrated into the half of original volume in 80 DEG C.
It is 65%(V/V that 8 alcohol precipitations add concentration in concentrated solution) edible ethanol makes alcohol concn in mixed system reach 55%(V/V) more than, place 12h for 5 DEG C and carry out alcohol precipitation, press filtration obtains filter residue.Adding concentration in filter residue is 95%(V/V) edible ethanol makes alcohol concn in mixed system reach 70%(V/V), stir 1h with the impurity in abundant stripping pectin, press filtration must be wet pectin.
After 9 press filtration alcohol precipitations, solution press filtration must be wet pectin.
10 dry wet pectin in 50 ~ 60 DEG C of oven dry, pulverize to obtain dry fruit glue.
Wet pectin color clear obtained as stated above, paler colour after dry, wherein galacturonic acid content reaches 65.2%.

Claims (1)

1. from fermentation haw thorn wine pomace, extract a method for pectin, it is characterized in that comprising the steps:
1) Hawthorn Fruit Wine pomace after fermentation is wrapped, add deionized water according to the ratio of pomace and water 1 ~ 2:2m/m, distill out hawthorn alcohol, filtering separation distillation residue and raffinate;
2) according to the ratio of distillation residue and water 1:1m/m, deionized water is added in distillation residue, collecting by filtration filtrate after 85 ~ 95 DEG C of stirring and leaching 1h;
3) by step 1) gained vinasse and step 2) filtrate of collecting mixing, 4500r/min is centrifugal, and 10min obtains supernatant liquor;
4) in supernatant liquor, add washing granulated active carbon, to supernatant liquor, contain washing granulated active carbon concentration is 1% ~ 5%m/v; Be heated to 60 ~ 80 DEG C of decolouring 30 ~ 90min; Filtering separation gac, obtains the colourless permeate of clear;
5) filtrate obtains concentrated solution in the half that 80 DEG C are concentrated into original volume;
6) in concentrated solution, add concentration is that 65%V/V edible ethanol makes alcohol concn in mixed system reach more than 55%V/V, and place 12h for 5 DEG C and carry out alcohol precipitation, press filtration obtains filter residue; Adding concentration in filter residue is that 95%V/V edible ethanol makes alcohol concn in mixed system reach 70%V/V, and stir 1h with the impurity in abundant stripping pectin, press filtration must be wet pectin;
7) wet pectin in 50 ~ 60 DEG C of oven dry, pulverize to obtain dry fruit glue.
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CN104316382B (en) * 2014-11-13 2017-10-27 光明乳业股份有限公司 A kind of detection method of preprocess method and pectin
CN105461824A (en) * 2016-02-17 2016-04-06 李嘉 Method for extracting low-fat pectin from passion fruit wine pomace
CN106632725B (en) * 2017-01-10 2019-06-11 涟源康麓生物科技有限公司 A method of separating water soluble pectin from pectin starting material rinsing liquid
CN110923090A (en) * 2018-09-20 2020-03-27 山东皇尊庄园山楂酒有限公司 Extraction method of hawthorn pectin and brewing method of hawthorn wine
CN109337790B (en) * 2018-09-30 2022-04-12 广西壮族自治区中国科学院广西植物研究所 Method for simultaneously preparing fruit original vinegar and pectin by taking pectin-rich fruits as raw materials
CN112159485B (en) * 2019-09-20 2022-12-30 山东皇尊庄园山楂酒有限公司 Hawthorn pectin extraction process and hawthorn product
CN110724289A (en) * 2019-11-28 2020-01-24 安阳工学院 Method for preparing edible film rich in hawthorn pectin and gelatin
CN112210022B (en) * 2020-11-12 2021-05-18 山东农业大学 Preparation method of low-methoxyl hawthorn pectin

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