CN105348394B - A kind of purification process of the grade particles of cornstarch 3 - Google Patents
A kind of purification process of the grade particles of cornstarch 3 Download PDFInfo
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- CN105348394B CN105348394B CN201510811973.8A CN201510811973A CN105348394B CN 105348394 B CN105348394 B CN 105348394B CN 201510811973 A CN201510811973 A CN 201510811973A CN 105348394 B CN105348394 B CN 105348394B
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Abstract
The invention discloses a kind of purification process of the grade particles of cornstarch 3, by cornstarch grain according to size be divided into greatly (>15 μm), in (10 15 μm) and it is small (<10 μm) three parts, including prepare starch suspension, stir, the centrifugation of 85% glycerine water solution, the big amylum body of Collection and conservation, 55% glycerine water solution are centrifuged, in Collection and conservation and the step such as small starch grains.The advantage of this method is good, easy to operate purification effect, the saving time, with low cost, can provide technical support to study the physicochemical property of cornstarch different size amylum body, contribute to the processing and application of cornstarch.
Description
Technical field
The present invention relates to the purification art of different size amylum body, more particularly to cornstarch different size particle is pure
Change method.
Background technology
The semi-crystalline particles structure that amylum body is made up of amylose and amylopectin, is synthesized in amyloplaste, is to plant
Important ergastic substances in object.The size of amylum body is to influence an important parameter of its functional characteristic, different size of shallow lake
Powder is either all endowed different purposes in food service industry or non-food industries.Granular size can putting down with amylum body
Equal particle diameter, the average value of short axle and major axis, maximum gauge, volume etc. are represented, according to different plant origins, amylum body size
Scope from 0.5 μm to 100 μm, such as tous-les-mois grain diameter be up to 100 μm；Farina grain is 15-75 μm；
Cornstarch grain is 5-20 μm；Rice fecula grain is 3-8 μm.
Size and amylose content, gelatinization point, Expansion Potential and water binding ability of different plant origin amylum bodies etc.
Starch physicochemical property is significantly correlated, and different size of amylum body shows different structural and functional characteristics.As barley is formed sediment
The bulky grain of powder includes the amylose of smaller, less branch, and its amylopectin includes more Type B long-chain branch；Ma Ling
The short grained particle diameter of sweet potato starch is 5-20 μm, and middle particle is 25-40 μm, and bulky grain is 40-85 μm, and as particle diminishes, it is gelatinized
Temperature is raised and heat content is reduced；The amylose content and gelatinization heat content of wheaten starch bulky grain are all higher than little particle.Except this it
Outside, the size of amylum body can also influence the quality of seed, and such as the barley seed rich in small starch grains is unsuitable for brewageing processing, and fits
In making paper and cosmetics；Barley seed rich in big amylum body is adapted to brewage processing.
Corn is annual gramineae herbaceous plant, is important cereal crops and feed resource, is also whole world total yield
Measure highest cereal crops.Corn is to manufacture one of important source material of starch, and starch accounts for 70% or so of corn seed dry weight, main
To be present in the form of starch grains in endosperm, the quality to corn seed has a great impact.The form of corn starch granules
It is similar, but the difference in size of different amylum bodies is obvious.
Different size of cornstarch grain is purified well, it is necessary to select a kind of efficient starch separation purification technique.
This technology be able to will not only have no amylum body to be divided into different particle size ranges and starch loss is reduced (especially with omitting
It is small starch grains), also to keep the dispersity and integrality (not being gelatinized also without mechanical damage) of particle.At present,
Existing many scholars are isolated and purified using various separating and purifying technologies to different size of amylum body, such as：1. by by
Corn with normal shape and obvious Unimodal Distribution and farina grain are respectively divided into of different sizes by level natural sedimentation
Four parts and five parts；2. the amylum body of Wheat Endosperm is divided into by of different sizes two by the screen cloth in 10 μm of apertures
Point；3. by centrifugal settling method, (medium is：Sucrose-the aqueous solution, maltose-aqueous solution or Precoll cell separations liquid) will be small
Amylum body in wheat germ breast is divided into two parts of different sizes.But all there are some defects in above several method：1. step by step certainly
The separating effect of right sedimentation is preferable, but a) amount of separating starch grain is seldom every time, because to control the concentration of amylum body to exist
2mg/mL, to ensure that sedimentation follows Stokes' law, causes the amount of starch obtained every time not enough；B) separation per one-level needs
Take considerable time, to ensure the purity of every one-level；2. crossing sieve method separating effect is not good, it is impossible to separate different size amylum body
Open；3. centrifugal settling method can largely separating starch grain, but a) every part of sucrose-aqueous solution, maltose-aqueous solution separation is formed sediment
Powder purity is not high；B) very well, purity is very high for the separating effect of Precoll cell separations liquid, but separating liquid is expensive, no
Suitable for a large amount of separating starch grain.In summary, we need badly existing amylum body isolation and purification method is improved with it is excellent
Change, overcome disadvantages described above, invent a kind of purification process of cornstarch different size particle, for research different size amylum body
Characteristic and its application provide technical support.
The content of the invention
In order to overcome the shortcomings of existing amylum body purification process, the amylum bodies at different levels of high-purity are obtained, the invention provides
A kind of purification process of cornstarch different size particle.
The purpose of the present invention can be reached by following measures：
A kind of purification process of the grade particles of cornstarch 3, it comprises the following steps：
(1) starch suspension is prepared：Native cornstarch and glycerine-water mixed solution of glycerine volumetric concentration 80~90% are mixed
After conjunction, be made into mass concentration be 1~5% starch suspension and stir；
(2) centrifuge：The starch suspension carries out 2~10min of centrifugation after mixing with 50~150g, is then demultiplex out for pure
Change the supernatant for neutralizing small starch grains, and solid；The sweet of glycerine volumetric concentration 80~90% is added into the solid isolated
Oil-water mixed solution is simultaneously fully mixed, and repeats the centrifugation in this step, separation and glycerine-water mixing is added into solid
The operation of solution and mixing 3~6 times, finally centrifuges 2~10min with 50~150g by the suspension of mixing, isolates for purifying
The supernatant of small starch grains is neutralized, and for purifying the solid of big amylum body；
(3) big amylum body is collected：To for purifying the solid of big amylum body and middle addition distilled water and mixing, in 5500~
6500g centrifuge 5~15min, remove supernatant, the solid centrifuged out is repeated in this step add distilled water mix and from
The operation of heart removing supernatant 3~6 times, the solid finally given is big amylum body；
(4) centrifuge：By being used for of being isolated in step (2) purify the supernatant for neutralizing small starch grains in 5500~
6500g centrifuges 5~15min, isolates glycerine-water mixed solution of supernatant, and glycerine body is added into the solid centrifuged out
Glycerine-water mixed solution of product concentration 50~60% is made into starch suspension and fully mixed, and 2~10min is centrifuged with 50~150g,
The supernatant for purifying small starch grains, and solid is then demultiplex out；Glycerine volumetric concentration is added into the solid isolated
50~60% glycerine-water mixed solution is simultaneously fully mixed, and repeats to centrifuge 2~10min, separation in this step with 50~150g
Supernatant and solid and the operation 3 added 50~60% glycerine-water mixed solution into the solid isolated and fully mixed
~6 times, suspension is finally centrifuged into 2~10min with 50~150g, the supernatant for purifying small starch grains, Yi Jiyong is isolated
The solid of amylum body in purifying；
(5) amylum body in collecting：That is isolated into step (4) is used in purifying addition distillation in the solid of amylum body
Water, is sufficiently stirred for carrying out 5~15min of centrifugation after 5500~6500g, removes supernatant and obtain solid, this is repeated to the solid
Distilled water and stirring, the operation for centrifuging and removing supernatant 3~6 times is added in step, during the solid finally given is
Amylum body；
(6) small starch grains are collected：Being used for of being isolated into step (4) purify the supernatants of small starch grains in 5500~
6500g carries out 5~15min of centrifugation, isolates glycerine-water mixed solution of supernatant, adds and steams into the solid centrifuged out
Distilled water, is sufficiently stirred for carrying out 5~15min of centrifugation after 5500~6500g, removes supernatant and obtain solid, the solid is repeated
Distilled water and stirring, the operation for centrifuging and removing supernatant 3~6 times is added in this step, the solid finally given is
Small starch grains；
(7) amylum body is preserved：Obtained big amylum body, middle amylum body and small starch grains are taken off with absolute ethyl alcohol repeatedly respectively
Water, then dries, crushes.
In a kind of preferred scheme, in step (1), the mass volume ratio of native cornstarch and glycerine-water mixed solution
For 1：Glycerine volumetric concentration is 85% in 35~45g/mL, glycerine-water mixed solution, and the mass concentration of the starch suspension is 2
~3%.
In a kind of preferred scheme, in step (2), isolate for purify neutralize small starch grains supernatant before from
Heart operating condition is：100g centrifuges 5min；The volumetric concentration of glycerine is 85% in the glycerine-water mixed solution；Corn original is formed sediment
The mass volume ratio of glycerine-water mixed solution of the powder with being added every time into the solid isolated is 1：35~45g/mL；Repeat
The operation for carrying out the centrifugation in this step, separate and glycerine-water mixed solution being added into solid and mix 4~5 times；Isolate
It is for purifying the centrifugally operated condition before the supernatant for neutralizing small starch grains：100g centrifuges 5min.
In a kind of preferred scheme, the glycerine-water mixed solution added in step (2) is partially or completely from step
(4) glycerine-water mixed solution for the supernatant isolated after being centrifuged first in.
In a kind of preferred scheme, in step (3), native cornstarch is 1 with the mass volume ratio of each distilled water：35
~45g/mL；Centrifugally operated condition in the step is：6000g centrifuges 10min；This step is repeated to the solid centrifuged out
It is middle to add the operation 4~5 times that distilled water mixed and be centrifuged off supernatant.
In a kind of preferred scheme, in step (4), the centrifugally operated bar for purifying the supernatant for neutralizing small starch grains
Part is：6000g centrifuges 10min；The volumetric concentration of glycerine is 55% in glycerine-water mixed solution in the step, is used every time
Glycerine-water mixed solution and native cornstarch volume mass ratio be 35~45：1mL/g；Isolate for purifying small starch
Grain supernatant before centrifugally operated condition be：100g centrifuges 5min；Repeat in this step with 100g centrifugations 5min, in separation
Clear liquid and solid and the operation adding 55% glycerine-water mixed solution into the solid isolated and fully mix 4~5 times；
Isolate for purify small starch grains supernatant before centrifugally operated condition be：100g centrifuges 5min.
In a kind of preferred scheme, the glycerine-water mixed solution added in step (4) is partially or completely from step
(6) centrifuge for purify small starch grains supernatant after glycerine-water mixed solution of supernatant for isolating.
In a kind of preferred scheme, in step (5), each consumption of distilled water and the volume mass ratio of native cornstarch
For 35~45：1mL/g；Centrifugally operated condition in the step is：6000g centrifuges 10min；Repeat the addition distillation in this step
The operation of water and stirring, centrifugation and removing supernatant 4~5 times.
In a kind of preferred scheme, in step (6), each consumption of distilled water and the volume mass ratio of native cornstarch
For 35~45：1mL/g；Centrifugally operated condition in the step is：6000g centrifuges 10min；Repeat the addition distillation in this step
The operation of water and stirring, centrifugation and removing supernatant 4~5 times.
In a kind of preferred scheme, in step (7), the process of each absolute ethyl alcohol dehydration is：Amylum body is immersed in
In absolute ethyl alcohol, it is sufficiently stirred for centrifuging 10min after 6000g, removes supernatant；In the step 2~3 are dehydrated with absolute ethyl alcohol
It is secondary；Drying temperature is 35~45 DEG C, and 100 mesh sieves are crossed after crushing.
Cornstarch grain according to particle size be divided into big amylum body (>15 μm), middle amylum body (10-15 μm) and small starch grains
(<10 μm) three parts, this method can be directly separated out the grade particles of cornstarch 3 by simple step.
A kind of present invention purification process of the specific grade particles of cornstarch 3 presented below, comprises the following steps：
(1) starch suspension is prepared：1.0g native cornstarchs are weighed respectively in 6 50mL plastic round bottom centrifuge tubes, at 6
It is each in centrifuge tube to add the Glycerine-Aqueous Solutions of 40mL 85%, it is made into the starch suspension that concentration is 2.5%；
(2) stir：The starch suspension in centrifuge tube is fully mixed by the way of glass bar is gently mixed；
(3) 85% Glycerine-Aqueous Solutions are centrifuged：
1. centrifuge：6 centrifuge tubes are centrifuged simultaneously, centrifuge 5min with 100g, supernatant is carefully drawn with pipette to one
In beaker；
2. 85% Glycerine-Aqueous Solution is supplemented：6 centrifuge tubes respectively add the Glycerine-Aqueous Solutions of 40mL 85%, again using glass
The mode that glass rod is gently mixed fully mixes the starch suspension in centrifuge tube；
3. repeat step 1. and 2. totally 5 times (1. the 5th only carries out step)；
(4) big amylum body is collected：
1. clean：Each in 6 centrifuge tubes to add 40mL distilled water, the mode being gently mixed with glass bar is by centrifuge tube
Starch suspension fully mix, 6000g centrifugation 10min, remove supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：Collect the precipitation in 6 centrifuge tubes, as big amylum body；
(5) 55% Glycerine-Aqueous Solutions are centrifuged：
1. collect：Supernatant in beaker is precipitated with 6000g centrifugations 10min, amylum body and small starch grains in being
Mixture；
2. starch suspension is prepared：The mixture of middle amylum body and small starch grains is sub-packed in 6 50mL plastic round bottom centrifugations
Guan Zhong, it is each in 6 centrifuge tubes to add the Glycerine-Aqueous Solutions of 40mL 55%, it is made into starch suspension；
3. stir：The starch suspension in centrifuge tube is fully mixed by the way of glass bar is gently mixed；
4. centrifuge：6 centrifuge tubes are centrifuged simultaneously, centrifuge 5min with 100g, supernatant is carefully drawn with pipette to one
In beaker；
5. 55% Glycerine-Aqueous Solution is supplemented：6 centrifuge tubes respectively add the Glycerine-Aqueous Solutions of 40mL 55%, again using glass
The mode that glass rod is gently mixed fully mixes the starch suspension in centrifuge tube；
6. repeat step 4. and 5. totally 5 times (4. the 5th only carries out step)；
(6) amylum body in collecting：
1. clean：Each in 6 centrifuge tubes to add 40mL distilled water, the mode being gently mixed with glass bar is by centrifuge tube
Starch suspension fully mix, 6000g centrifugation 10min, remove supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：The precipitation in 6 centrifuge tubes is collected, amylum body in being；
(7) small starch grains are collected：
1. centrifuge：Supernatant in beaker is precipitated with 6000g centrifugations 10min；
2. clean：Precipitation is sub-packed in 6 centrifuge tubes, it is each to add 40mL distilled water, the side being gently mixed with glass bar
Formula fully mixes the starch suspension in centrifuge tube, 6000g centrifugation 10min, removes supernatant；
3. repeat step 2. 5 times, glycerine is fully washed away；
4. collect：Collect the precipitation in 6 centrifuge tubes, as small starch grains；
(8) amylum body is preserved：The big of collection, the small starch of neutralization are dehydrated 2 times with absolute ethyl alcohol respectively, 40 DEG C of drying are used
Mortar wears into starch powder, crosses 100 mesh sieves, and drier is saved backup；Wherein absolute ethyl alcohol dehydration requirement be：
1. starch need to be immersed in absolute ethyl alcohol；
2. it is slowly stirred 10min with magnetic stirring apparatus；
3. 6000g centrifuges 10min after dehydration every time, removes supernatant.
Compared with existing fecula purifying method, advantage of the invention is that：
(1) a kind of purification process of cornstarch different size amylum body has been invented.
(2) can once purify much starch grain, take it is very short, overcome natural sedimentation purifying starch amount step by step it is few, consumption
The defect of duration.
(3) purification effect is very good, and every partial starch grain purity of purifying is very high, overcomes crossing sieve method purification effect not
It is good, the sucrose-aqueous solution, maltose-not high defect of aqueous solution centrifugal settling method purifying starch grain purity.
(4) low cost is purified, it is adaptable to which high-volume is purified, and overcomes Precoll cell separation liquid centrifugal settling method prices
Expensive defect.
(5) offer reference is isolated and purified for different size amylum body, contributes to researcher further to analyze starch
The structural and functional characteristic of grain, processing and application to amylum body have great importance.
Brief description of the drawings
Fig. 1 is a kind of purifying schematic flow sheet of different size cornstarch grain of the present invention；
Fig. 2 is the ordinary optical microscope photo of amylum bodies at different levels after purification；
Fig. 3 is the electron scanning micrograph of amylum bodies at different levels after purification.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1：The purifying of common corn starch grain：(flow entirely purified is shown in Fig. 1)
(1) starch suspension is prepared：
1. 85% Glycerine-Aqueous Solution is prepared：212.5mL pure glycerin+37.5mL distilled water, is fully mixed；
2. 1.0g conventional corns ative starch (buying in Penford companies) is weighed respectively to centrifuge in 6 50mL plastic round bottom
Manage in (A groups centrifuge tube), it is each in 6 centrifuge tubes to add the Glycerine-Aqueous Solutions of 40mL 85%, it is made into the starch that concentration is 2.5%
Suspension；
(2) stir：The starch suspension 5min in centrifuge tube is persistently stirred by the way of glass bar is gently mixed, is made
Amylum body is dispersed in Glycerine-Aqueous Solution；
(3) 85% Glycerine-Aqueous Solutions are centrifuged：
1. centrifuge：6 centrifuge tubes are centrifuged simultaneously immediately, centrifuge 5min with 100g, supernatant is carefully drawn with pipette to one
In beaker, small starch grains are neutralized for purifying；
2. the suspension in beaker is sub-packed in 6 new 50mL plastic round bottom centrifuge tubes (B groups centrifuge tube), 6000g from
Heart 10min, the supernatant of collection is 85% Glycerine-Aqueous Solution；
3. 85% Glycerine-Aqueous Solution is supplemented：6 centrifuge tubes (A groups centrifuge tube) respectively add the Glycerine-Aqueous Solutions of 40mL 85%
(85% Glycerine-Aqueous Solution 2. reclaimed using step), persistently stirs centrifuge tube by the way of glass bar is gently mixed again
In starch suspension 5min, amylum body is dispersed in Glycerine-Aqueous Solution；
4. repeat step 1. -3. totally 5 times (1. the 5th only carries out step)；
(4) big amylum body is collected：
1. clean：It is each in 6 centrifuge tubes (A groups centrifuge tube) to add 40mL distilled water, the side being gently mixed with glass bar
Formula persistently stirs starch suspension 5min, 6000g the centrifugation 10min in centrifuge tube, removes supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：Collect the precipitation in 6 centrifuge tubes, as big amylum body；
(5) 55% Glycerine-Aqueous Solutions are centrifuged：
1. 55% Glycerine-Aqueous Solution is prepared：137.5mL pure glycerin+112.5mL distilled water, is fully mixed；
2. starch suspension is prepared：It is each in 6 centrifuge tubes (B groups centrifuge tube) to add the Glycerine-Aqueous Solutions of 40mL 55%, match somebody with somebody
Into starch suspension；
3. stir：The starch suspension 5min in centrifuge tube is persistently stirred by the way of glass bar is gently mixed, is made
Amylum body is dispersed in Glycerine-Aqueous Solution；
4. centrifuge：6 centrifuge tubes are centrifuged simultaneously immediately, centrifuge 5min with 100g, supernatant is carefully drawn with pipette
Into a beaker；
5. the suspension in beaker is sub-packed in 6 new 50mL plastic round bottom centrifuge tubes (C groups centrifuge tube), 6000g from
Heart 10min, the supernatant of collection is 55% Glycerine-Aqueous Solution；
6. 55% Glycerine-Aqueous Solution is supplemented：6 centrifuge tubes (B groups centrifuge tube) respectively add the Glycerine-Aqueous Solutions of 40mL 55%
(85% Glycerine-Aqueous Solution 5. reclaimed using step), persistently stirs centrifuge tube by the way of glass bar is gently mixed again
In starch suspension 5min, amylum body is dispersed in Glycerine-Aqueous Solution；
7. repeat step 4. -6. totally 5 times (4. the 5th only carries out step)；
(6) amylum body in collecting：
1. clean：It is each in 6 centrifuge tubes (B groups centrifuge tube) to add 40mL distilled water, the side being gently mixed with glass bar
Formula persistently stirs starch suspension 5min, 6000g the centrifugation 10min in centrifuge tube, removes supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：The precipitation in 6 centrifuge tubes is collected, amylum body in being；
(7) small starch grains are collected：
1. clean：It is each in 6 centrifuge tubes (C groups centrifuge tube) to add 40mL distilled water, the side being gently mixed with glass bar
Formula persistently stirs starch suspension 5min, 6000g the centrifugation 10min in centrifuge tube, removes supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：Collect the precipitation in 6 centrifuge tubes, as small starch grains；
(8) amylum body is preserved：
1. it is dehydrated：By collection it is big, neutralize small starch grains and be dehydrated that 2 times (starch need to be immersed in anhydrous with absolute ethyl alcohol respectively
In ethanol, with magnetic stirring apparatus moderate-speed mixer 10min, 6000g centrifugations 10min after dehydration, removes supernatant every time)；
2. dry：40 DEG C of dry 2d, starch powder is worn into mortar, crosses 100 mesh sieves, and drier is saved backup.
Embodiment 2：The purifying of amylomaize grain：(flow entirely purified is shown in Fig. 1)
(1) starch suspension is prepared：
1. 85% Glycerine-Aqueous Solution is prepared：212.5mL pure glycerin+37.5mL distilled water, is fully mixed；
2. 1.0g high straight-chain maizes ative starch is weighed respectively (to buy in Australian Penford companies, numbering：Gelose
50) in 6 50mL plastic round bottom centrifuge tubes (A groups centrifuge tube), each glycerine of 40mL 85%-water-soluble of adding in 6 centrifuge tubes
Liquid, is made into the starch suspension that concentration is 2.5%；
(2) stir：The starch suspension 5min in centrifuge tube is persistently stirred by the way of glass bar is gently mixed, is made
Amylum body is dispersed in Glycerine-Aqueous Solution；
(3) 85% Glycerine-Aqueous Solutions are centrifuged：
1. centrifuge：6 centrifuge tubes are centrifuged simultaneously immediately, centrifuge 5min with 100g, supernatant is carefully drawn with pipette to one
In beaker, small starch grains are neutralized for purifying；
2. the suspension in beaker is sub-packed in 6 new 50mL plastic round bottom centrifuge tubes (B groups centrifuge tube), 6000g from
Heart 10min, the supernatant of collection is 85% Glycerine-Aqueous Solution；
3. 85% Glycerine-Aqueous Solution is supplemented：6 centrifuge tubes respectively add the Glycerine-Aqueous Solutions of 40mL 85% (using step 2.
85% Glycerine-Aqueous Solution reclaimed), the starch suspension in centrifuge tube is persistently stirred by the way of glass bar is gently mixed again
5min, makes amylum body be dispersed in Glycerine-Aqueous Solution；
4. repeat step 1. -3. totally 5 times (1. the 5th only carries out step)；
(4) big amylum body is collected：
1. clean：It is each in 6 centrifuge tubes (A groups centrifuge tube) to add 40mL distilled water, the side being gently mixed with glass bar
Formula persistently stirs starch suspension 5min, 6000g the centrifugation 10min in centrifuge tube, removes supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：Collect the precipitation in 6 centrifuge tubes, as big amylum body；
(5) 55% Glycerine-Aqueous Solutions are centrifuged：
1. 55% Glycerine-Aqueous Solution is prepared：137.5mL pure glycerin+112.5mL distilled water, is fully mixed；
2. starch suspension is prepared：It is each in 6 centrifuge tubes (B groups centrifuge tube) to add the Glycerine-Aqueous Solutions of 40mL 55%, match somebody with somebody
Into starch suspension；
3. stir：The starch suspension 5min in centrifuge tube is persistently stirred by the way of glass bar is gently mixed, is made
Amylum body is dispersed in Glycerine-Aqueous Solution；
4. centrifuge：6 centrifuge tubes are centrifuged simultaneously immediately, centrifuge 5min with 100g, supernatant is carefully drawn with pipette
Into a beaker；
5. the suspension in beaker is sub-packed in 6 new 50mL plastic round bottom centrifuge tubes (C groups centrifuge tube), 6000g from
Heart 10min, the supernatant of collection is 55% Glycerine-Aqueous Solution；
6. 55% Glycerine-Aqueous Solution is supplemented：6 centrifuge tubes respectively add the Glycerine-Aqueous Solutions of 40mL 55% (using step 5.
85% Glycerine-Aqueous Solution reclaimed), the starch suspension in centrifuge tube is persistently stirred by the way of glass bar is gently mixed again
5min, makes amylum body be dispersed in Glycerine-Aqueous Solution；
7. repeat step 4. -6. totally 5 times (4. the 5th only carries out step)；
(6) amylum body in collecting：
1. clean：It is each in 6 centrifuge tubes (B groups centrifuge tube) to add 40mL distilled water, the side being gently mixed with glass bar
Formula persistently stirs starch suspension 5min, 6000g the centrifugation 10min in centrifuge tube, removes supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：The precipitation in 6 centrifuge tubes is collected, amylum body in being；
(7) small starch grains are collected：
1. clean：It is each in 6 centrifuge tubes (C groups centrifuge tube) to add 40mL distilled water, the side being gently mixed with glass bar
Formula persistently stirs starch suspension 5min, 6000g the centrifugation 10min in centrifuge tube, removes supernatant；
2. repeat step 1. 5 times, glycerine is fully washed away；
3. collect：Collect the precipitation in 6 centrifuge tubes, as small starch grains；
(8) amylum body is preserved：
1. it is dehydrated：By collection it is big, neutralize small starch grains and be dehydrated that 2 times (starch need to be immersed in anhydrous with absolute ethyl alcohol respectively
In ethanol, with magnetic stirring apparatus moderate-speed mixer 10min, 6000g centrifugations 10min after dehydration, removes supernatant every time)；
2. dry：40 DEG C of dry 2d, starch powder is worn into mortar, crosses 100 mesh sieves, and drier is saved backup.
It is big between the three partial starch grain of purifying with the form and size of observation by light microscope cornstarch grain after purification
Small difference substantially, and per partial starch grain form, uniform in size, purity is very high, illustrate that purification effect is fine (Fig. 2)；With
SEM observes form, size and the surface topography of cornstarch grain after purification, finds the shape of the grain per partial starch
State, uniform in size, surface is very smooth, illustrates that purge process does not cause to damage to every partial starch grain, purification effect (figure very well
3)；The average grain diameter of cornstarch grain after purification is determined with laser fineness gage, starch intergranulars at different levels have significant difference,
It apparent can distinguish, illustrate purification effect very well (table 1).
The average grain diameter of the different size cornstarch grain of table 1
Wherein, D (3,2)：Surface area weighted average diameter, D (4,3)：Volume weighted average diameter.
Claims (10)
1. a kind of purification process of the grade particles of cornstarch 3, it is characterised in that comprise the following steps：
(1) starch suspension is prepared：Native cornstarch is mixed with glycerine-water mixed solution of glycerine volumetric concentration 80~90%
Afterwards, be made into mass concentration be 1~5% starch suspension and stir；
(2) centrifuge：The starch suspension carries out 2~10min of centrifugation after mixing with 50~150g, is then demultiplex out for purifying
Neutralize the supernatant of small starch grains, and solid；Added into the solid isolated the glycerine of glycerine volumetric concentration 80~90%-
Water mixed solution is simultaneously fully mixed, and repeats the centrifugation in this step, separation and glycerine-water mixed solution is added into solid
And the operation 3~6 times mixed, the suspension of mixing is finally centrifuged into 2~10min with 50~150g, isolates and is neutralized for purifying
The supernatant of small starch grains, and for purifying the solid of big amylum body；
(3) big amylum body is collected：Distilled water is added into the solid for purifying big amylum body and is mixed, in 5500~6500g
5~15min is centrifuged, supernatant is removed, the solid centrifuged out is repeated to add distilled water mixing in this step and centrifugation is removed
The operation 3~6 times of supernatant is gone, the solid finally given is big amylum body；
(4) centrifuge：By isolated in step (2) be used for purify neutralize small starch grains 5500~6500g of supernatant from
5~15min of the heart, isolates glycerine-water mixed solution of supernatant, and glycerine volumetric concentration 50 is added into the solid centrifuged out
~60% glycerine-water mixed solution is made into starch suspension and fully mixed, and centrifuges 2~10min with 50~150g, then separates
Go out the supernatant for purifying small starch grains, and solid；Glycerine volumetric concentration 50~60% is added into the solid isolated
Glycerine-water mixed solution and fully mix, repeat 2~10min is centrifuged with 50~150g, separated for purifying in this step
The supernatant and solid of small starch grains and added into the solid isolated 50~60% glycerine-water mixed solution and fully mix
Even operation 3~6 times, finally centrifuges 2~10min with 50~150g by suspension, isolates the supernatant for purifying small starch grains
Liquid, and the solid for amylum body in purifying；
(5) amylum body in collecting：Distilled water is added in the solid for amylum body in purifying isolated into step (4), is filled
Divide stirring to carry out 5~15min of centrifugation after 5500~6500g, remove supernatant and obtain solid, the solid is repeated in this step
Add distilled water and stirring, centrifugation and remove the operation 3~6 times of supernatant, the solid finally given is middle amylum body；
(6) small starch grains are collected：By the supernatant for being used to purify small starch grains isolated in step (4) in 5500~6500g
5~15min of centrifugation is carried out, glycerine-water mixed solution of supernatant is isolated, distilled water is added into the solid centrifuged out,
It is sufficiently stirred for carrying out 5~15min of centrifugation after 5500~6500g, removes supernatant and obtain solid, this step is repeated to the solid
In add distilled water and stirring, centrifugation and remove the operation 3~6 times of supernatant, the solid finally given is small starch
Grain；
(7) amylum body is preserved：Obtained big amylum body, middle amylum body and small starch grains are dehydrated with absolute ethyl alcohol repeatedly respectively,
Then dry, crush.
2. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (1), corn
Ative starch is 1 with the mass volume ratio of glycerine-water mixed solution：Glycerine volume is dense in 35~45g/mL, glycerine-water mixed solution
Spend for 85%, the mass concentration of the starch suspension is 2~3%.
3. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (2), separation
Go out and be for purifying the centrifugally operated condition before the supernatant for neutralizing small starch grains：100g centrifuges 5min；Glycerine-the water is mixed
The volumetric concentration for closing glycerine in solution is 85%；Native cornstarch is mixed with the glycerine-water added every time into the solid isolated
The mass volume ratio for closing solution is 1：35~45g/mL；Repeat the centrifugation in this step, separation and added into solid sweet
The operation of oil-water mixed solution and mixing 4~5 times；Isolate for purifying the centrifugation behaviour before the supernatant for neutralizing small starch grains
It is as condition：100g centrifuges 5min.
4. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that added in step (2)
Glycerine-water mixed solution is molten partially or completely from the glycerine-water mixing for the supernatant isolated after being centrifuged first in step (4)
Liquid.
5. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (3), corn
Ative starch is 1 with the mass volume ratio of each distilled water：35~45g/mL；Centrifugally operated condition in the step is：6000 g
Centrifuge 10min；The solid centrifuged out is repeated to add the operation that distilled water mixed and be centrifuged off supernatant in this step
4~5 times.
6. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (4), be used for
The centrifugally operated condition of supernatant that purifying neutralizes small starch grains is：6000g centrifuges 10min；Glycerine-water mixing in the step
The volumetric concentration of glycerine is 55%, the glycerine-water mixed solution and the volume mass ratio of native cornstarch used every time in solution
For 35~45：1mL/g；Isolate for purify small starch grains supernatant before centrifugally operated condition be：100 g are centrifuged
5min；Repeat being added with 100g centrifugations 5min, separation supernatant and solid and into the solid isolated in this step
55% glycerine-water mixed solution and the operation that fully mixes 4~5 times；Isolate before the supernatant for purifying small starch grains
Centrifugally operated condition is：100g centrifuges 5min.
7. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that added in step (4)
Glycerine-water mixed solution partially or completely from step (6) centrifuge for purify small starch grains supernatant after isolate
Supernatant glycerine-water mixed solution.
8. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (5), distillation
Each consumption of water and the volume mass ratio of native cornstarch are 35~45：1mL/g；Centrifugally operated condition in the step is：
6000g centrifuges 10min；Repeat to add distilled water and stirring, centrifugation and the operation 4~5 for removing supernatant in this step
It is secondary.
9. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (6), distillation
Each consumption of water and the volume mass ratio of native cornstarch are 35~45：1mL/g；Centrifugally operated condition in the step is：
6000g centrifuges 10min；Repeat to add distilled water and stirring, centrifugation and the operation 4~5 for removing supernatant in this step
It is secondary.
10. the purification process of the grade particles of cornstarch 3 according to claim 1, it is characterised in that in step (7), often
The process of secondary absolute ethyl alcohol dehydration is：Amylum body is immersed in absolute ethyl alcohol, is sufficiently stirred for centrifuging 10 min after 6000g,
Remove supernatant；It is dehydrated 2~3 times with absolute ethyl alcohol in the step；Drying temperature is 35~45 DEG C, and 100 mesh sieves are crossed after crushing.
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