CN108477618A - A kind of controllable method for preparing of pectin nanometer selenium - Google Patents
A kind of controllable method for preparing of pectin nanometer selenium Download PDFInfo
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- CN108477618A CN108477618A CN201810109724.8A CN201810109724A CN108477618A CN 108477618 A CN108477618 A CN 108477618A CN 201810109724 A CN201810109724 A CN 201810109724A CN 108477618 A CN108477618 A CN 108477618A
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- pectin
- nanometer selenium
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- selenium
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000011669 selenium Substances 0.000 title claims abstract description 67
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 67
- 239000001814 pectin Substances 0.000 title claims abstract description 42
- 229920001277 pectin Polymers 0.000 title claims abstract description 42
- 235000010987 pectin Nutrition 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229940091258 selenium supplement Drugs 0.000 claims abstract description 66
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims abstract description 16
- 235000015921 sodium selenite Nutrition 0.000 claims abstract description 16
- 229960001471 sodium selenite Drugs 0.000 claims abstract description 11
- 239000011781 sodium selenite Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 9
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 9
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 9
- 238000000502 dialysis Methods 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 229940082569 selenite Drugs 0.000 claims description 4
- MCAHWIHFGHIESP-UHFFFAOYSA-L selenite(2-) Chemical compound [O-][Se]([O-])=O MCAHWIHFGHIESP-UHFFFAOYSA-L 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 14
- 239000002245 particle Substances 0.000 abstract description 9
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- 150000004676 glycans Chemical class 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 5
- 239000005017 polysaccharide Substances 0.000 description 5
- 239000003381 stabilizer Substances 0.000 description 5
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 3
- 229920001661 Chitosan Polymers 0.000 description 2
- 235000004237 Crocus Nutrition 0.000 description 2
- 241000596148 Crocus Species 0.000 description 2
- -1 D- galacturonic acid residues Polysaccharide Chemical class 0.000 description 2
- 235000013878 L-cysteine Nutrition 0.000 description 2
- 239000004201 L-cysteine Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001473 noxious effect Effects 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 description 1
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 208000002177 Cataract Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000010412 Glaucoma Diseases 0.000 description 1
- 229920002581 Glucomannan Polymers 0.000 description 1
- 208000019926 Keshan disease Diseases 0.000 description 1
- 229920002752 Konjac Polymers 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229920002385 Sodium hyaluronate Polymers 0.000 description 1
- 235000004298 Tamarindus indica Nutrition 0.000 description 1
- 240000004584 Tamarindus indica Species 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 229940046240 glucomannan Drugs 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 208000021267 infertility disease Diseases 0.000 description 1
- 231100000567 intoxicating Toxicity 0.000 description 1
- 230000002673 intoxicating effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LGZXYFMMLRYXLK-UHFFFAOYSA-N mercury(2+);sulfide Chemical compound [S-2].[Hg+2] LGZXYFMMLRYXLK-UHFFFAOYSA-N 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 235000020124 milk-based beverage Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 201000008482 osteoarthritis Diseases 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 1
- 229940010747 sodium hyaluronate Drugs 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/16—Inorganic salts, minerals or trace elements
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/10—General methods of cooking foods, e.g. by roasting or frying
- A23L5/19—General methods of cooking foods, e.g. by roasting or frying using chemicals before or during cooking, e.g. liquid cooking media other than water or oil; Cooking using inert particles, e.g. fluidised bed cooking
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Food Science & Technology (AREA)
- Nutrition Science (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Mycology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a kind of controllable method for preparing of pectin nanometer selenium, belong to the green preparing technical field of nano material.Include the following steps：Distilled water is added in a certain amount of pectin powder, and after stirring, centrifugation, filter membrane, 4 DEG C of refrigerators are stood overnight, and are balanced, and obtains the aqueous pectin solution that mass fraction is 0.1%；The sodium selenite solution of 0.1mol/L is added in 0.1% aqueous pectin solution, 25 DEG C of stirring 1min；The ascorbic acid solution of 0.2mol/L is added dropwise, is stirred for 24 hours under normal temperature and pressure；Mixed liquor dialysis 48h, freeze-drying, obtained red powder is pectin nanometer selenium, by the volume for controlling sodium selenite solution, the nanometer selenium of different-grain diameter size can be obtained, therefore is that a kind of environmentally protective, simple and practicable, raw material sources are abundant, nanometer selenium particle size is controllable, stability is good, water-soluble and good biocompatibility preparation method.
Description
Technical field
The present invention relates to the green preparing technical field of nano material, more particularly to a kind of pectin is as stabilizer and dispersion
The method of agent controllable preparation nanometer selenium.
Background technology
Selenium is important trace element needed by human, has a variety of physiology work(such as enhancing immunity of organisms, anticancer, diseases prevention
Energy.It is the 60 μ g/d of μ g/d~200 that the selenium intake standard of normal population is recommended by Chinese Soclety of Nutrition, and world health group is defined as 40
The μ of μ g/d~100 g/d.Selenium intake deficiency can lead to the imbalance of human body vitals function, cause Kaschin-Beck disease, Keshan disease, white
The diseases such as cataract or glaucoma, infertile.Selenium-supply mainly has two kinds of forms of inorganic selenium and Organic Selenium.However, selenium is in optium concentration and intoxicating
Margin of safety between concentration is very narrow, therefore develops emphasis and hot spot that less toxic, efficient selenium source is selemium nutrition research.
Compared with inorganic selenium and Organic Selenium, zeroth order red nano selenium has better bioavailability and higher biology living
Property, and there is lower toxicity, it is current it has been found that the minimum selenium form of toxicity, can be directly absorbed by the body profit
With with good application prospect in the exploitation of selenium-supply product.Health ministry approved nanometer selenium capsule is health food
(hygienic food and health number 1998 the 134th).But it is usually unstable by nanometer selenium prepared by reduction method, it is easy to happen aggregation, is caused
Its lower bioactivity and bioavailability, and then limit practical application.Food-grade polysaccharide is due to good biology
Compatibility, biodegradability and wide spectrum biological activity and functionality prepare nanometer selenium as stabilizer and dispersant.Mesh
The preceding more carbohydrates and their derivatives reported include mainly：Chitosan, carboxymethyl chitosan, konjaku glucomannan, Arabic gum, Portugal
Glycan, Sodium Hyaluronate, carboxymethyl cellulose, tamarind seed polysaccharide, oyster polysaccharide.It is worth noting that, Chinese invention patent (CN
104825484 A；CN104800240 A；CN105520953 A；CN 102145174 B；102603396 B of CN) also disclose
The preparation methods of several polysaccharide and its derivates nanometer selenium.
Pectin is a kind of natural, acid macromolecular for being aggregated into α (1 → 4) glycosidic bond by D- galacturonic acid residues
Polysaccharide is widely present in the plants group food such as fruit and vegetable, is a kind of important dietary fiber sources, has to health more
Kind important function.Pectin has extensively in the food industry as gelling agent, stabilizer, thickener, emulsifier, texture modifying agent
Using.Due to containing a large amount of carboxyl, hydroxyl, methoxyl group isoreactivity group in pectin molecule, stabilizer, reducing agent have been used as it
Carry out green syt noble metal nano particles with oxidant.
Through retrieval, report is yet there are no about the method using pectin as stabilizer and dispersant controllable preparation nanometer selenium at present
Road.
Invention content
The purpose of the present invention is to provide a kind of controllable method for preparing of pectin nanometer selenium, this method is simple and practicable, cost
It is cheap, operability is strong, and entire reaction is without noxious material or environmental contaminants, and can realize continuous large-scale production, particle
The controllable environment-friendly preparation method thereof of size.Also, the pectin nanometer selenium prepared has, and stability is good, particle diameter distribution is uniform, divides
Dissipate the good feature of property.
Used technical solution is the present invention in order to achieve the above objectives：A kind of controllable method for preparing of pectin nanometer selenium,
It carries out as steps described below：
(1) a certain amount of pectin powder is weighed, distilled water is added, after stirring, 5000rpm, 20min centrifugation,
Filter membrane, 4 DEG C of refrigerators are stood overnight, balance, obtain the aqueous pectin solution that mass fraction is 0.1%；
(2) the selenite solution that different volumes molar concentration is 0.1mol/L is added to the pectin that step (1) obtains
In aqueous solution, 1min is stirred under room temperature；
(3) aqueous ascorbic acid is added dropwise to liquid-transfering gun in the mixed liquor that step (2) obtains, under normal temperature and pressure
Stirring is for 24 hours；
(4) the mixed liquor distilled water dialysis 48h that step (3) obtains, freeze-drying, obtained red powder is different grains
The pectin nanometer selenium of diameter size.
Step (1) described pectin is from orange peel, apple skin and other rich pectous agricultural product or processing of farm products
Any one of waste, the water phase filter membrane that the filter membrane is 0.45 μm；
Step (2) described selenite is sodium selenite, the sodium selenite and pectin solution volume ratio be 0.3~
15.5：200 (v/v), the room temperature are 25 DEG C；
The molar concentration of step (3) described ascorbic acid is 0.2mol/L, the ascorbic acid and pectin solution volume ratio
It is 1.0：200(v/v)；
Step (4) described dialysis process is to use bag filter, and the molecule interception of bag filter is 3500Da.
The present invention has advantageous effect.The present invention is led to using pectin, sodium selenite as raw material under normal temperature and pressure conditions
It crosses ascorbic acid reduction and is made pectin nanometer selenium, it is environmentally protective without noxious material or environmental contaminants in entire reaction process.It is logical
The dosage for crossing control sodium selenite solution, can obtain the controllable pectin nanometer selenium of particle size.Operating procedure is simple and practicable, former
Expect abundance, the nanometer selenium of preparation has good stability, water solubility and biocompatibility, easy to implement continuous extensive
Production, and can be applied to, as a kind of novel selenium supplementary form in fruit juice, acidic milk drink, have good answer in field of food
Use foreground.
Description of the drawings
Fig. 1 is the TEM figures of nanometer selenium made from the embodiment of the present invention 1；
Fig. 2 is the TEM figures of nanometer selenium made from the embodiment of the present invention 2；
Fig. 3 is the TEM figures of nanometer selenium made from the embodiment of the present invention 3；
Fig. 4 is the TEM figures of nanometer selenium made from the embodiment of the present invention 4；
Fig. 5 is the TEM figures of nanometer selenium made from the embodiment of the present invention 5；
Fig. 6 is the TEM figures of nanometer selenium made from the embodiment of the present invention 6.
Specific implementation mode
The present invention is described in further detail below by embodiment, it should be pointed out that embodiment described below purport
Convenient for the understanding of the present invention, and any restriction effect is not played to it.
Comparative example：
Chinese invention patent CN106219501A discloses " a kind of selenium nano particle and preparation method thereof ".One of which selenium
The preparation method of nano particle is：15g apple pectins are added in the sodium selenite solution of the 0.1mol/L of 1000mL, constantly to molten
L-cysteine is added in liquid and reaches 0.4mol/L until reaching the final concentration of L-cysteine, by the mixture of gained at 50 DEG C
Lower stirring 10 hours.Then sodium ion and the L-cysteine of oxidation are removed by dialysis process, are contained in the obtained solution
There is the amorphous selenium particle that apple pectin is protected.Obtained amorphous selenium particle passes through transmission electron microscope observing, selenium nano particle
From 20-40nm etc., average-size size is 30nm.
Embodiment 1：
The sodium selenite solution of 0.3mL 0.1mol/L is added to the aqueous pectin solution that 200mL mass fractions are 0.1%
In, 25 DEG C of stirring 1min are added dropwise the ascorbic acid solution of 1.0mL 0.2mol/L, are reacted under normal temperature and pressure for 24 hours, dialysis
48h, freeze-drying, obtains nanometer selenium solid powder.
The nanometer selenium dispersion of above-mentioned preparation is obtained into the pectin nanometer selenium water that mass concentration is 0.5mg/mL in deionized water
Solution, nanometer selenium solution colour are in light yellow, observe its TEM figures, as shown in Figure 1, nanometer selenium pattern is spherical in shape, have small part poly-
Collection, average grain diameter 53nm.
Embodiment 2：
The present embodiment is substantially the same manner as Example 1, the difference is that the volume of 0.1mol/L sodium selenites is
15.5mL。
Nanometer selenium solution colour is in brown color, the nanometer selenium TEM figures of above-mentioned preparation is observed, as shown in Fig. 2, nanometer selenium pattern
Spherical in shape, particle diameter distribution is uniform, average grain diameter 51nm.
Embodiment 3：
The present embodiment is substantially the same manner as Example 1, the difference is that the volume of 0.1mol/L sodium selenites is
6.0mL。
Nanometer selenium solution colour is in brick-red, the nanometer selenium TEM figures of above-mentioned preparation is observed, as shown in figure 3, nanometer selenium pattern
In monodisperse, uniform spherical structure, particle diameter distribution is uniform, average grain diameter 40nm.
Embodiment 4：
The present embodiment is substantially the same manner as Example 1, the difference is that the volume of 0.1mol/L sodium selenites is
1.0mL。
Nanometer selenium solution colour is in crocus, the nanometer selenium TEM figures of above-mentioned preparation is observed, as shown in figure 4, nanometer selenium pattern
Most of spherical in shape, less oval, average grain diameter 48nm.
Embodiment 5：
The present embodiment is substantially the same manner as Example 1, the difference is that the volume of 0.1mol/L sodium selenites is
2.5mL。
Nanometer selenium solution colour is in Chinese red, the nanometer selenium TEM figures of above-mentioned preparation is observed, as shown in figure 5, nanometer selenium is in ball
Shape structure, particle diameter distribution is uniform, average grain diameter 45nm.
Embodiment 6：
The present embodiment is substantially the same manner as Example 1, the difference is that the volume of 0.1mol/L sodium selenites is
11.5mL。
Nanometer selenium solution colour is in crocus, the nanometer selenium TEM figures of above-mentioned preparation is observed, as shown in fig. 6, nanometer selenium pattern
It is spherical in shape, average grain diameter 47nm.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the above is only
It for specific embodiments of the present invention, is not intended to restrict the invention, all any modifications made in the spirit of the present invention
With improve etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of controllable method for preparing of pectin nanometer selenium, it is characterised in that carry out as steps described below：
(1) a certain amount of pectin powder is weighed with assay balance, distilled water, after stirring, 5000rpm, 20min is added
Centrifugation, filter membrane, 4 DEG C of refrigerators are stood overnight, and are balanced, are obtained aqueous pectin solution；
(2) the selenite solution of different volumes is added in the aqueous pectin solution that step (1) obtains, is stirred under room temperature
1min；
(3) aqueous ascorbic acid is added dropwise to liquid-transfering gun in the mixed liquor that step (2) obtains, is stirred under normal temperature and pressure
24h；
(4) the mixed liquor distilled water dialysis 48h that step (3) obtains, freeze-drying, obtained red powder is that different-grain diameter is big
Small pectin nanometer selenium.
2. a kind of controllable method for preparing of pectin nanometer selenium according to claim 1, it is characterised in that wherein step (1) institute
Any of the pectin stated in orange peel, apple skin and other rich pectous agricultural product or processing of farm products waste
Kind；The mass fraction of the aqueous pectin solution is 0.1%；The water phase filter membrane that the filter membrane is 0.45 μm.
3. a kind of controllable method for preparing of pectin nanometer selenium according to claim 1, it is characterised in that wherein step (2) institute
The selenite stated is sodium selenite；The molar concentration of the sodium selenite is 0.1mol/L；The sodium selenite and pectin are molten
Liquid volume ratio is 0.3~15.5：200(v/v)；The room temperature is 25 DEG C.
4. a kind of controllable method for preparing of pectin nanometer selenium according to claim 1, it is characterised in that wherein step (3) institute
The molar concentration for the ascorbic acid stated is 0.2mol/L；The volume ratio of the ascorbic acid and pectin solution is 1.0：200.
5. a kind of controllable method for preparing of pectin nanometer selenium according to claim 1, it is characterised in that wherein step (4) institute
The dialysis process stated is to use bag filter；The molecule interception of the bag filter is 3500Da.
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