CN104086667A - Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction - Google Patents
Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction Download PDFInfo
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Abstract
The invention relates to a technology for preparing high-standard pectin from citrus fruit peel residues. The citrus fruit peel residues are employed as a raw material. Through processes such as pre-process of the raw material and the like, activity of original pectinase in the peels is destroyed. Cellulase is added to carry out an enzymolysis reaction to cellulose in cell walls of peel cells, and then a pectin crude extract is extracted by an ultrasonic-assisted acid liquid method. The pectin crude extract is subjected to a precipitation process through alcohol, a washing process and a vacuum drying process to obtain a high-quality pectin finish product. The biological enzymolysis method and the ultrasonic-assisted acid liquid method are employed for extracting pectin from residual residues of citrus fruit peels after processing. Through the extraction technology, an extraction time is significantly shortened and negative influences of a strong acid condition and a long-time heating process on degradation of pectin are overcome, thereby increasing a yield of pectin. Pectin prepared through the method is good in color and is high in purity and yield.
Description
Technical field
The present invention relates to natural product extraction manufacture field, is exactly a kind of method of utilizing ultrasonic-assisted extraction to prepare citrus skin slag pectin.
Background technology
Pectin is a kind of high molecular polymer, is extensively present in higher plant cell wall and intercellular substance, is generally white or pale yellow powder, odorless, and taste is micro-sweet, is slightly with tart flavour, is insoluble to the organic solvent such as ethanol, methyl alcohol, is dissolved in hot water, is slightly soluble in cold water.Because pectin derives from natural extract, nontoxic, safe and reliable, there is good gelation and emulsifying stability, Chang Zuowei jelling agent, stablizer, emulsifying agent, thickening material, organize the natural additive for foodstuffs such as modifying agent, usually should be in food-processing and Chemicals.In addition, that pectin also has is antibacterial, detumescence, removing toxic substances, antidiarrheal, the effect such as hypotensive, is also widely used in field of medicaments.Along with the development research of functional polysaccharide, pectin, as water-soluble dietary fibre, is more and more subject to the attention of scholar and processing industry.
The present invention, taking citrus peel residue as raw material, therefrom extracts pectin and not only increases economic efficiency, and is more conducive to protection of the environment, realizes processing of farm products waste deep development and resource circulation utilization.
Ultrasonic wave refers to the mechanical wave of range of frequency at 20KHz, and velocity of wave is generally 1500m/s, wavelength be 0.01-10cm. it formed by the compressional wave of a series of density interphases, and propagate to surrounding by liquid medium.Ultrasonic wave can be destroyed tissue and the cell of citrus peel residue, solvent is penetrated in histocyte, the pectic substance being conducive to wherein leaches and separates, this is because hyperacoustic effect is a physical process, in leaching process, occur without chemical reaction, can not make pectin structure and character change, improve leaching velocity, shorten extraction time.
Summary of the invention
The object of the present invention is to provide a kind of energy Reaction time shorten, improve the quality of products, be convenient to industrialization operation and utilize ultrasonic-assisted extraction to prepare the method for citrus skin slag pectin.
Above-mentioned purpose realizes by following scheme:
Utilize ultrasonic-assisted extraction to prepare a method for citrus skin slag pectin, it is characterized in that:
Citrusfruit skin slag is removed to impurity and the enzyme pre-treatment of going out, add cellulase to carry out enzymolysis, recycling ultrasonic-assisted extraction equipment, it is acid regulating extracting solution PH, carry out ultrasonic wave auxiliary acid water extraction pectin, extract is carried out centrifugal, filter, get supernatant liquor, vacuum concentration, the ethanol precipitation of 95% left and right fully stirs simultaneously, washing is also centrifugal, and collecting precipitation thing, vacuum lyophilization obtain pectin finished product.
A kind of described method of utilizing ultrasonic-assisted extraction to prepare citrus skin slag pectin, is characterized in that: comprise the following steps:
(1) with after 35-55 DEG C of warm water rinsing for several times, be then heated to 85-95 DEG C, insulation 10-20 min; Use again after 35-55 DEG C of warm water rinsing for several times, dry, be crushed to 80 order left and right, the citrusfruit skin slag that must remove impurity and go out after enzyme;
(2) before enzyme-added, regulate pH condition at 3.5-5.5, control solid-liquid ratio at 1:20-30 simultaneously, add cellulase 0.1-0.5U/g, hydrolysis temperature is 35-65 DEG C, enzymolysis time 65-90min, and boiling water bath 85-95 DEG C after enzymolysis completes, the enzyme that goes out about time 5min is lived;
(3) utilize the acid extraction liquid of the combination of organic acid and mineral acid to adjust pH1.8-2.4, ultrasonic-assisted extraction 45-75min, insulation 60-85 DEG C, ultrasonic power is 225-250W;
(4) rotating speed 4200-6000r/min, centrifugal 15-25min, retains supernatant liquor, is centrifugate;
(5) centrifugate is concentrated into the 4-6% of original volume under temperature 45-65 DEG C condition, is cooled to rapidly room temperature;
(6), to the ethanol that adds 95% left and right that is equivalent to its 2-4 times volume in concentrated solution, keep 4 DEG C of left and right of temperature, precipitation 1-2 h, with centrifugal 10min left and right, 3600rmp left and right, through filtered through gauze, then through absolute ethanol washing 1-2 time, obtain the hygrometric state pectin after alcohol precipitation;
(7) by the pre-freeze 24-36 h below-18 DEG C of the hygrometric state pectin after alcohol precipitation, then vacuum lyophilization, pectin power-product obtained.
Utilize ultrasonic-assisted extraction to prepare a method for citrus skin slag pectin, it is characterized in that: the acid extraction liquid of described organic acid and the combination of mineral acid by hydrochloric acid, sulfuric acid, sulfurous acid, citric acid etc. one or more combination and obtain;
Utilize ultrasonic-assisted extraction to prepare a method for citrus skin slag pectin, it is characterized in that: the acid extraction liquid of described organic acid and the combination of mineral acid is obtained by mixing in 1:1:1:1 ratio by hydrochloric acid, sulfuric acid, sulfurous acid, citric acid.
Beneficial effect of the present invention is:
(1) taking the citrusfruit skin slag of processing waste as raw material, there is raw materials cost cheap, can realize the increment utilization of discarded peel residue, and avoid contaminate environment.
(2) original polygalacturonase in passivation pericarp, can prevent the decomposition of pectin in leaching process, thereby improves pectin yield.
(3) utilize the Mierocrystalline cellulose in cellulose degraded pericarp membrane wall, make better stripping of pectin.
(4) ultrasonic-assisted extraction, is conducive to the efficient stripping of pectin substance, shortens extraction time, improves pectin extraction rate.
Embodiment
Now, taking laboratory implementation as example, non-limiting examples is described below:
Embodiment 1,
Enzymatic hydrolysis condition is determined: before enzyme-added, first use citric acid-sodium citrate (damping fluid) to regulate potential of hydrogen (controlled enzymatic hydrolysis pH is at 3.5-5.5), meanwhile, strictly control solid-liquid ratio in 1:20-30 scope.Add cellulase 0.1-0.5U/g, hydrolysis temperature is 35-65 DEG C, enzymolysis time 65-90min.
Raw materials pretreatment: citrus peel residue is carried out to two step process: remove impurity and the enzyme (original polygalacturonase in skin slag) that goes out.Object is: remove the materials such as glucosides a large amount of in pericarp, starch, pigment, acids, salt.Method is: with warm water (35-55 DEG C) rinsing repeatedly, and then heating (85-95 DEG C), insulation 10-20 min, makes original polygalacturonase passivation; Use again warm water (35-55 DEG C) rinsing repeatedly, further impurity elimination, oven dry, pulverizing (80 order), for subsequent use.
Enzymolysis process: accurately take 10.000g through pretreated citrus peel residue, by " enzymatic hydrolysis condition is determined " solid-liquid ratio, and add distilled water to stir, enzymolysis.The enzyme that goes out rapidly after enzymolysis completes (boiling water bath 85-95 DEG C, time 5min) alive.
Pectin extraction, separation: utilize the combination of organic acid and mineral acid (to comprise: one or more the combination such as hydrochloric acid, sulfuric acid, sulfurous acid, citric acid, in 1:1:1:1 ratio) acid extraction liquid (adjust pH1.8-2.4), ultrasonic-assisted extraction 45-75min, insulation 60-85 DEG C, ultrasonic power is 225-250W.With rotating speed 4200-6000r/min, centrifugal 15-25min, retains supernatant liquor, is centrifugate again.Centrifugate is rotated the 4-6% that is evaporated to original volume under temperature 45-65 DEG C condition, is cooled to rapidly room temperature.
Pectin precipitation, dry: to 95% ethanol that adds 2-4 times of volume in concentrated solution, keep 4 DEG C of temperature, precipitation 1-2 h, with the centrifugal 10min of 3600rmp, through filtered through gauze, then uses absolute ethanol washing 1-2 time, obtains hygrometric state pectin.By the pre-freeze 24-36 h below-18 DEG C of the pectin after alcohol precipitation, then vacuum lyophilization, pectin power-product obtained.
?
Embodiment 2,
1, raw materials pretreatment: oranges and tangerines are processed to remaining skin slag and suitably process, mainly comprise two steps: remove impurity and the enzyme that goes out, by the mode of rinsing and blanching, raw material pericarp is carried out to pre-treatment.Object is: remove the materials such as glucosides a large amount of in pericarp, starch, pigment, acids, salt.Method is: with warm water (35-55 DEG C) rinsing repeatedly, and then heating (85-95 DEG C), insulation 10-20 min, makes original polygalacturonase passivation in pericarp; Use again warm water (35-55 DEG C) rinsing repeatedly, further impurity elimination, oven dry, pulverizing (80 order), for subsequent use.
2, enzymolysis: before enzyme-added, first regulate potential of hydrogen (controlled enzymatic hydrolysis pH condition is at 3.5-5.5) by citric acid-sodium citrate, meanwhile, strictly control solid-liquid ratio in 1:20-30 scope.Add cellulase 0.1-0.5U/g, hydrolysis temperature is 35-65 DEG C, enzymolysis time 65-90min.The enzyme that goes out rapidly after enzymolysis completes (boiling water bath 85-95 DEG C, time 5min) alive.
3, acid solution is extracted: utilize the combination of organic acid and mineral acid (to comprise: the combination of one or more acid such as hydrochloric acid, sulfuric acid, sulfurous acid, citric acid, in 1:1:1:1 ratio) acid extraction liquid (adjust pH1.8-2.4), ultrasonic-assisted extraction 45-75min, insulation 60-85 DEG C, ultrasonic power is 225-250W.
4, centrifugal: rotating speed 4200-6000r/min, centrifugal 15-25min, retains supernatant liquor, is centrifugate.
5, vacuum concentration: centrifugate is rotated the 4-6% that is evaporated to original volume under temperature 45-65 DEG C condition, is cooled to rapidly room temperature.
6, alcohol precipitation: to 95% ethanol that adds 2-4 times of volume in concentrated solution, keep 4 DEG C of temperature, precipitation 1-2 h, with the centrifugal 10min of 3600rmp, through filtered through gauze, then through absolute ethanol washing 1-2 time, obtains hygrometric state pectin.
7, dry: by the pre-freeze 24-36 h below-18 DEG C of the pectin after alcohol precipitation, then vacuum lyophilization, obtain pectin power-product.
Embodiment 3,
A kind of described method of utilizing ultrasonic-assisted extraction to prepare citrus skin slag pectin, comprises the following steps:
(1) with after 45 DEG C of warm water rinsings 3 times, be then heated to 95 DEG C, insulation 10 min; Use again after 35 DEG C of warm water rinsings 2 times, dry, be crushed to 80 orders, the citrusfruit skin slag that must remove impurity and go out after enzyme;
(2) before enzyme-added, regulating pH condition is 4.5, controls solid-liquid ratio at 1:25 simultaneously, adds cellulase 0.4U/g, and hydrolysis temperature is 45 DEG C, enzymolysis time 68min, and 95 DEG C of boiling water baths after enzymolysis completes, the time 5min enzyme that goes out is lived;
(3) utilize the acid extraction liquid of the combination of organic acid and mineral acid to adjust pH2, ultrasonic-assisted extraction 60min, is incubated 65 DEG C, and ultrasonic power is 250W;
(4) rotating speed 6000r/min, centrifugal 25min, retains supernatant liquor, is centrifugate;
(5) centrifugate is concentrated into 5% of original volume under 5 DEG C of conditions of temperature, is cooled to rapidly room temperature;
(6) to adding 95% the ethanol that is equivalent to its 3 times of volumes in concentrated solution, keep 4 DEG C of temperature, precipitation 2 h, with the centrifugal 10min of 3600rmp, through filtered through gauze, then through absolute ethanol washing 2 times, obtain the hygrometric state pectin after alcohol precipitation;
(7) by the hygrometric state pectin after alcohol precipitation at-15 DEG C of pre-freeze 36 h, then vacuum lyophilization, obtains pectin power-product.
Claims (4)
1. utilize ultrasonic-assisted extraction to prepare a method for citrus skin slag pectin, it is characterized in that:
Citrusfruit skin slag is removed to impurity and the enzyme pre-treatment of going out, add cellulase to carry out enzymolysis, recycling ultrasonic-assisted extraction equipment, it is acid regulating extracting solution PH, carry out ultrasonic wave auxiliary acid water extraction pectin, extract is carried out centrifugal, filter, get supernatant liquor, vacuum concentration, the ethanol precipitation of 95% left and right fully stirs simultaneously, washing is also centrifugal, and collecting precipitation thing, vacuum lyophilization obtain pectin finished product.
2. a kind of method of utilizing ultrasonic-assisted extraction to prepare citrus skin slag pectin according to claim 1, is characterized in that: comprise the following steps:
(1) with after 35-55 DEG C of warm water rinsing for several times, be then heated to 85-95 DEG C, insulation 10-20 min; Use again after 35-55 DEG C of warm water rinsing for several times, dry, be crushed to 80 order left and right, the citrusfruit skin slag that must remove impurity and go out after enzyme;
(2) before enzyme-added, regulate pH condition at 3.5-5.5, control solid-liquid ratio at 1:20-30 simultaneously, add cellulase 0.1-0.5U/g, hydrolysis temperature is 35-65 DEG C, enzymolysis time 65-90min, and boiling water bath 85-95 DEG C after enzymolysis completes, the enzyme that goes out about time 5min is lived;
(3) utilize the acid extraction liquid of the combination of organic acid and mineral acid to adjust pH1.8-2.4, ultrasonic-assisted extraction 45-75min, insulation 60-85 DEG C, ultrasonic power is 225-250W;
(4) rotating speed 4200-6000r/min, centrifugal 15-25min, retains supernatant liquor, is centrifugate;
(5) centrifugate is concentrated into the 4-6% of original volume under temperature 45-65 DEG C condition, is cooled to rapidly room temperature;
(6), to the ethanol that adds 95% left and right that is equivalent to its 2-4 times volume in concentrated solution, keep 4 DEG C of left and right of temperature, precipitation 1-2 h, with centrifugal 10min left and right, 3600rmp left and right, through filtered through gauze, then through absolute ethanol washing 1-2 time, obtain the hygrometric state pectin after alcohol precipitation;
(7) by the pre-freeze 24-36 h below-18 DEG C of the hygrometric state pectin after alcohol precipitation, then vacuum lyophilization, pectin power-product obtained.
3. utilize ultrasonic-assisted extraction to prepare the method for citrus skin slag pectin according to one kind of claim 1, it is characterized in that: the acid extraction liquid of described organic acid and the combination of mineral acid by hydrochloric acid, sulfuric acid, sulfurous acid, citric acid etc. one or more combination and obtain.
4. utilize ultrasonic-assisted extraction to prepare the method for citrus skin slag pectin according to one kind of claim 1, it is characterized in that: the acid extraction liquid of described organic acid and the combination of mineral acid is obtained by mixing in 1:1:1:1 ratio by hydrochloric acid, sulfuric acid, sulfurous acid, citric acid.
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| CN104686887A (en) * | 2015-02-13 | 2015-06-10 | 邵素英 | Beauty maintaining honey paste and preparation method thereof |
| CN104686888A (en) * | 2015-02-13 | 2015-06-10 | 邵素英 | Honey cream capable of improving skin functions and preparation method of honey cream |
| CN105566512A (en) * | 2015-12-14 | 2016-05-11 | 山东省果树研究所 | Extracting method of persimmon fruit pectin |
| CN105777935A (en) * | 2016-03-11 | 2016-07-20 | 华中农业大学 | Preparation method of high-emulsibility mango peel pectin |
| CN105906741A (en) * | 2016-06-02 | 2016-08-31 | 华南理工大学 | Method for extracting pectin from waste sisal residues |
| CN106666519A (en) * | 2016-12-12 | 2017-05-17 | 湖北工业大学 | Fat substitute containing active ingredients of pomelo peel, as well as preparation method and application thereof |
| CN106722476A (en) * | 2016-12-12 | 2017-05-31 | 湖北工业大学 | Fat substitute and preparation method and application containing orange peel active component |
| CN107266608A (en) * | 2017-07-25 | 2017-10-20 | 孔科喜 | The extracting method of orange peel pectin |
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| CN108433113A (en) * | 2018-01-22 | 2018-08-24 | 华南理工大学 | A kind of method that ultrasonication prepares citrus fruit fibres |
| CN106146687B (en) * | 2016-09-28 | 2018-10-16 | 中国科学院重庆绿色智能技术研究院 | A kind of method of pectin in extraction citrus peel residue |
| CN109122842A (en) * | 2018-08-15 | 2019-01-04 | 邯郸学院 | A kind of jackfruit bacteriostasis, preservation spray and preparation method thereof |
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| CN113354755A (en) * | 2021-05-17 | 2021-09-07 | 淮北凯乐生物科技有限公司 | High-efficiency pectin extraction process |
| CN113773410A (en) * | 2021-10-12 | 2021-12-10 | 广东四国生物科技有限公司 | Method for extracting pectin from citrus residues |
| CN114656578A (en) * | 2022-04-22 | 2022-06-24 | 华南理工大学 | Method for preparing high-ester pectin rich in RG-I by enzyme-assisted method |
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| CN105566512B (en) * | 2015-12-14 | 2018-03-30 | 山东省果树研究所 | A kind of extracting method of persimmon fruit pectin |
| CN105566512A (en) * | 2015-12-14 | 2016-05-11 | 山东省果树研究所 | Extracting method of persimmon fruit pectin |
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