CN104086668B - A kind of method preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste - Google Patents
A kind of method preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste Download PDFInfo
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- CN104086668B CN104086668B CN201410259025.3A CN201410259025A CN104086668B CN 104086668 B CN104086668 B CN 104086668B CN 201410259025 A CN201410259025 A CN 201410259025A CN 104086668 B CN104086668 B CN 104086668B
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- neosynephrine
- pectin
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- ethanol
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Abstract
The present invention provides a kind of method utilizing citrus fruits industrial wood waste to prepare pectin coproduction Neosynephrine, and the extraction separating step of the method includes: extraction of being heated by the skin slag ethanol of citrus fruits industrial wood waste；Extract is centrifuged, obtains filtrate I and filtering residue；Regulating PH with hydrochloric acid after gained filtering residue water logging, centrifugal, centrifugal gained supernatant fluid filtrate is concentrated in vacuo (recycling design), then promotes precipitation with 95% ethanol: stand, centrifugal, obtains filtrate II and precipitate filtering residue；Gained precipitate filtering residue is vacuum dried, obtains pectin finished product；Filtrate II obtained as above and filtrate I are mixed, is concentrated in vacuo, remove the ethanol in extract, then be vacuum dried, obtain Neosynephrine finished product.The present invention is dissolved in ethanol based on Neosynephrine, the pectin characteristic insoluble in ethanol, devise new process route, this method can obtain Neosynephrine and two kinds of products of pectin simultaneously, ensures simultaneously, and improves the yield of pectin and Neosynephrine, equipment is simple, easily operated, product keeps natural prodcuts characteristic, and quality is high.
Description
Technical field
The present invention relates to the primary product manufacture field of food industry processing and natural drug, be exactly a kind of from Citrus chachiensis Hort.
The method preparing pectin coproduction Neosynephrine in Fructus Citri tangerinae class fruit industrial wood waste.
Background technology
Containing multiple effective one-tenth such as pectin, pigment, Neosynephrine, quintessence oils in citrus fruits industrial wood waste peel
Point.The comprehensive utilization of peel marc in recent years not yet causes enough attention, the most Citrus chachiensiss Hort. produced during Citrus procession
The residues such as Fructus Citri tangerinae class peel abandon because going rotten rotten, cause resource significant wastage, but also pollute environment.
Neosynephrine was synthesized by Germany scientist at first in nineteen twenty-seven,, nature is distributed in rutaceae Citrus aurantium Linn.
In leaf and dry young fruit and Cactaeous plants, also it is the principle active component of Chinese crude drug Pericarpium Citri Reticulatae Viride, Pericarpium Citri Reticulatae, Fructus Aurantii, Fructus Aurantii Immaturus, because of product
Kind, the place of production, the different Neosynephrine content differences of time of picking.Research shows: fruit gets over maturation, and Neosynephrine content is more
Low, typically in immature fruit, Neosynephrine content is higher.
Neosynephrine (synephrine) molecular formula is C9H13NO2,Molecular weight is 167.20, and structure is as it is shown in figure 1, Neosynephrine
Belonging to the ephedrines in alkaloid, there is phenolic hydroxyl group and amino in molecular structure simultaneously, therefore Neosynephrine has amphotericity,
Salt all can be combined into soda acid.Free Neosynephrine is soluble in organic solvent, is insoluble in water；Its acid salt and basic salt are the most readily soluble
Yu Shui, is insoluble in organic solvent.When strong acid, strong alkali ion exchange resin chromatography easily there is racemization in Neosynephrine.
Natural pectin is widely present in the fruit of higher plant, root, stem, leaf with Pectin, proto, pectin, the form of pectic acid
In, it is a kind of constituent of cell wall.Pectin is a kind of polysaccharide macromolecular compound, and its chemical constitution is more complicated, its
Primary structure is to be connected, by D mono-galactopyranosyluronic, the straight chain polymer formed by a-1,4-glycosidic bond.Poly-galactose
The carboxyl of aldehydic acid has esterification in various degree, the carboxyl of non-esterification to have the form of free acid or with forms such as potassium, sodium, calcium salts
Exist.The galacturonic acid main chain of pectin is also frequently accompanied by the side chains such as rhamnose, arabinose, galactose, xylose, trehalose.
The relative molecular mass of pectin from several ten thousand to hundreds of thousands.
Commodity pectin is the white or faint yellow nontoxic pulverulent solids of odorless, and mouthfeel stick-slip has hygroscopicity, affine with water
Power is extremely strong, soluble in water, and aqueous solution thickness, is slightly soluble in Diluted Alcohol, is practically insoluble in the organic solvents such as methanol, ethanol, ether.
Owing to pectin derives from plant extract, nontoxic, in the food industry frequently as additive.Owing to pectin has
There are the functional characteristics such as good gel, thickening, stable, emulsifying, therefore, are widely used to food, medicine, chemical industry, weaving etc.
Industry, has played positive effect to the life improving people.
Summary of the invention
It is an object of the invention to provide a kind of pectin coproduction Neosynephrine prepared from citrus fruits industrial wood waste
Method, for asking existing for the existing Technology of extraction pectin and Neosynephrine from citrus fruits industrial wood waste at present
Topic, proposing a kind of can be to extract pectin and the method for Neosynephrine simultaneously.
Above-mentioned purpose is realized by below scheme:
A kind of method preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste, it is characterised in that: include
Following steps:
(1), after citrus fruits industrial wood waste carries out enzyme denaturing and deimpurity pretreatment, pretreated raw material is obtained standby
With；
(2) raw material of pretreatment is added distilled water and the second that concentration is 90-95% of 3-5 times amount by solid-liquid ratio 1:20-30
Alcohol, is heated to 60-90 DEG C, extracts 1.5-2h, obtains leaching extract；
(3) above-mentioned leaching extract is centrifuged, obtains filtrate I and filtering residue；
(4) by the filter residue and drying of above-mentioned steps gained, it is crushed to about 60 mesh, adds distilled water by solid-liquid ratio 1:20-30,
Regulate PH to 1.8-2.4 with hydrochloric acid, stand 2-4h, be then centrifuged for, the supernatant after centrifugal is concentrated in vacuo, adds 2-
The concentration of 4 times of volumes is the ethanol of about 95%, places 1-3h, obtains filtrate II and precipitate filtering residue；
(5) the precipitate filtering residue of above-mentioned steps (4) gained is vacuum dried, obtains pectin finished product；
(6) the filtrate I that the filtrate II of step (4) gained obtains with step (3) is mixed, be concentrated in vacuo, the vacuum of gained
Concentrated solution, removes the ethanol in extract, liquid vacuum drying is concentrated in vacuo, obtains Neosynephrine finished product.
A kind of described method preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste, its feature exists
In:
The method of enzyme denaturing and deimpurity pretreatment is: citrus fruits industrial wood waste floats in the warm water of 35-55 DEG C
Wash 2-3 time, be then heated to 85-95 DEG C of insulation 10-20 min, make pectase be passivated；Again with 35-55 DEG C of warm water rinse
2-3 time, to wash away impurity further, dry, be crushed to, about 80 mesh, obtain pretreated raw material for standby.
The invention have the benefit that
(1) citrus fruits industrial wood waste refers to the leftover bits and pieces of processing of the citrus fruits such as Citrus, Fructus Citri Limoniae, Fructus Citri grandis
(or residue), the present invention had both made full use of raw material, avoided again the wasting of resources, polluted environment.
(2) making full use of industrial wood waste, during technological design, produces Neosynephrine and two kinds of products of pectin simultaneously, from
And it is substantially reduced production cost, increase the benefit.
(3) extraction process is simple, and quality is easily controlled, and method is reliable；
(4) extraction efficiency is high, and product stability is good
The present invention is dissolved in ethanol based on Neosynephrine, the pectin characteristic insoluble in ethanol, designs a new process route,
Make Neosynephrine major part dissolution in the leachate extracting pectin, obtain the most pectous Neosynephrine extracting solution, thus obtain height
The Neosynephrine product of quality.And, extract the filtering residue after Neosynephrine and can extract pectin further, carry alcohol deposition method with acid and extract fruit
Glue, does not interferes with the yield of pectin, and does not contains chemical reagent in finished product, makes product can keep natural prodcuts characteristic, is
A kind of most valuable green product.
Accompanying drawing explanation
Fig. 1 is Neosynephrine structure chart.
Detailed description of the invention
Now as a example by laboratory implementation, non-limiting examples is described below:
Embodiment 1,
After citrus fruits industrial wood waste carries out enzyme denaturing and deimpurity pretreatment, obtain pretreated raw material for standby；
Obtain pretreated raw material 50g, add distilled water by solid-liquid ratio 1:25, add the ethanol 200ml of 95%, be heated to 90
DEG C, to extract 1.5h, be then centrifuged 20min with centrifuge with 4200r/min rotating speed, the centrifugal liquid obtained becomes filtrate I.Filter
Slag plant pulverizer is ground into 60 mesh, adds distilled water by solid-liquid ratio 1:20-30, regulates PH to 1.9 with hydrochloric acid, stands 3h,
It is centrifuged 20min with centrifuge with 4200r/min afterwards, the supernatant fluid filtrate after centrifugal is concentrated in vacuo, adds 5 times of volumes
95% ethanol, places 3h, produces a large amount of precipitation, with 4200r/min rotating speed, above-mentioned standing liquid centrifuge is centrifuged 15min,
The centrifugal liquid obtained becomes filtrate II, and centrifugal after precipitate vacuum drying, obtain pectin finished product, weighing obtains total pectin and contains
Amount.Filtrate I and II is mixed, is concentrated in vacuo, remove the ethanol in extract, be then vacuum dried, obtain Neosynephrine finished product.
Embodiment 2,
A kind of method preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste, comprises the following steps:
(1) citrus fruits industrial wood waste rinses 3 times in the warm water of 55 DEG C, is then heated to 95 DEG C of insulations 20
Min, makes pectase be passivated；Again with 55 DEG C of warm water rinse 3 times, to wash away impurity further, dry, be crushed to 80 mesh, obtain pre-place
Raw material for standby after reason.
(2) raw material of pretreatment is added distilled water and the ethanol that concentration is 95% of 5 times amount, heating by solid-liquid ratio 1:30
To 60 DEG C, extract 2h, obtain leaching extract；
(3) above-mentioned leaching extract is centrifuged, obtains filtrate I and filtering residue；
(4) by the filter residue and drying of above-mentioned steps gained, it is crushed to 60 mesh, adds distilled water by solid-liquid ratio 1:30, use hydrochloric acid
Regulation PH to 2.4, stands 4h, is then centrifuged for, and is concentrated in vacuo by the supernatant after centrifugal, adds the concentration of 4 times of volumes
It is the ethanol of 95%, places 3h, obtain filtrate II and precipitate filtering residue；
(5) the precipitate filtering residue of above-mentioned steps (4) gained is vacuum dried, obtains pectin finished product；
(6) the filtrate I that the filtrate II of step (4) gained obtains with step (3) is mixed, be concentrated in vacuo, the vacuum of gained
Concentrated solution, removes the ethanol in extract, liquid vacuum drying is concentrated in vacuo, obtains Neosynephrine finished product.
Claims (2)
1. the method preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste, it is characterised in that: include with
Lower step:
(1), after citrus fruits industrial wood waste carries out enzyme denaturing and deimpurity pretreatment, pretreated raw material for standby is obtained；
(2) to pretreated raw material, add distilled water by solid-liquid ratio 1:20-30, add pretreated raw material 3-5 times amount
The ethanol that concentration is 90-95%, be heated to 60-90 DEG C, extract 1.5-2h, obtain leaching extract；
(3) above-mentioned leaching extract is centrifuged, obtains filtrate I and filtering residue；
(4) by the filter residue and drying of above-mentioned steps gained, it is crushed to 60 mesh, adds distilled water by solid-liquid ratio 1:20-30, adjust with hydrochloric acid
Joint pH to 1.8-2.4, stands 2-4h, is then centrifuged for, and is concentrated in vacuo by the supernatant after centrifugal, adds 2-4 times of volume
The ethanol that concentration is 95%, place 1-3h, obtain filtrate II and precipitate filtering residue；
(5) the precipitate filtering residue of above-mentioned steps (4) gained is vacuum dried, obtains pectin finished product；
(6) the filtrate I that the filtrate II of step (4) gained obtains with step (3) is mixed, be concentrated in vacuo, being concentrated in vacuo of gained
Liquid, removes the ethanol in extract, liquid vacuum drying is concentrated in vacuo, obtains Neosynephrine finished product.
A kind of side preparing pectin coproduction Neosynephrine from citrus fruits industrial wood waste the most according to claim 1
Method, it is characterised in that: the method for enzyme denaturing and deimpurity pretreatment is: citrus fruits industrial wood waste is in the temperature of 35-55 DEG C
Water rinses 2-3 time, is then heated to 85-95 DEG C of insulation 10-20 min, makes pectase be passivated；Again with 35-55 DEG C of warm water
Rinse 2-3 time, to wash away impurity further, dry, be crushed to 80 mesh, obtain pretreated raw material for standby.
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| US3622559A (en) * | 1967-11-01 | 1971-11-23 | Sunkist Growers Inc | Method for producing pectins having high resistance to breakage and high capability for gelling in the presence of calcium |
| CN101402577B (en) * | 2008-10-23 | 2011-07-20 | 浙江工商大学 | Method for extracting and separating levorotation-synephrine from green tangerine orange peel |
| CN101875703A (en) * | 2010-05-28 | 2010-11-03 | 砀山宇宁生物科技有限公司 | Method for extracting pectin and synephrine by utilizing peels and marc |
| CN103641932A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from orange peels |
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Inventor after: Ding Zhien Inventor after: Li Jingnan Inventor after: Zhang Jigang Inventor after: Ding Yu Inventor after: Xu Hao Inventor after: Fang Jie Inventor before: Ding Zhien Inventor before: Li Jingnan Inventor before: Zhang Jigang Inventor before: Ding Yu Inventor before: Xu Hao Inventor before: Fang Jie |
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Free format text: CORRECT: INVENTOR; FROM: DING ZHIEN LI QINGNAN ZHANG JIGANG DING YU XU HAO FANG JIE TO: DING ZHIEN LI JINGNAN ZHANG JIGANG DING YU XU HAO FANG JIE |
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