CN109601999A - A kind of lycopene nanometer powder and preparation method thereof - Google Patents
A kind of lycopene nanometer powder and preparation method thereof Download PDFInfo
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- CN109601999A CN109601999A CN201811296244.3A CN201811296244A CN109601999A CN 109601999 A CN109601999 A CN 109601999A CN 201811296244 A CN201811296244 A CN 201811296244A CN 109601999 A CN109601999 A CN 109601999A
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- lycopene
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- 229960004999 lycopene Drugs 0.000 title claims abstract description 163
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 title claims abstract description 162
- JEVVKJMRZMXFBT-XWDZUXABSA-N Lycophyll Natural products OC/C(=C/CC/C(=C\C=C\C(=C/C=C/C(=C\C=C\C=C(/C=C/C=C(\C=C\C=C(/CC/C=C(/CO)\C)\C)/C)\C)/C)\C)/C)/C JEVVKJMRZMXFBT-XWDZUXABSA-N 0.000 title claims abstract description 162
- 239000001751 lycopene Substances 0.000 title claims abstract description 162
- 235000012661 lycopene Nutrition 0.000 title claims abstract description 162
- ZCIHMQAPACOQHT-ZGMPDRQDSA-N trans-isorenieratene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/c1c(C)ccc(C)c1C)C=CC=C(/C)C=Cc2c(C)ccc(C)c2C ZCIHMQAPACOQHT-ZGMPDRQDSA-N 0.000 title claims abstract description 162
- OAIJSZIZWZSQBC-GYZMGTAESA-N lycopene Chemical compound CC(C)=CCC\C(C)=C\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C=C(/C)CCC=C(C)C OAIJSZIZWZSQBC-GYZMGTAESA-N 0.000 title claims abstract description 161
- 239000000843 powder Substances 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000007908 nanoemulsion Substances 0.000 claims abstract description 32
- 238000001694 spray drying Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000003860 storage Methods 0.000 abstract description 11
- 230000014759 maintenance of location Effects 0.000 abstract description 8
- 235000013305 food Nutrition 0.000 abstract description 7
- 235000021049 nutrient content Nutrition 0.000 abstract description 4
- 239000002245 particle Substances 0.000 description 49
- 238000002474 experimental method Methods 0.000 description 21
- 239000011858 nanopowder Substances 0.000 description 21
- 235000020122 reconstituted milk Nutrition 0.000 description 19
- 229920002472 Starch Polymers 0.000 description 18
- 235000019698 starch Nutrition 0.000 description 18
- 239000008107 starch Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- -1 such as Vc Substances 0.000 description 12
- 239000006210 lotion Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 230000031700 light absorption Effects 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 6
- 229930006000 Sucrose Natural products 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000005720 sucrose Substances 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 5
- 241000227653 Lycopersicon Species 0.000 description 5
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 238000005457 optimization Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 239000001054 red pigment Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- YBJHBAHKTGYVGT-ZKWXMUAHSA-N (+)-Biotin Chemical compound N1C(=O)N[C@@H]2[C@H](CCCCC(=O)O)SC[C@@H]21 YBJHBAHKTGYVGT-ZKWXMUAHSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000013361 beverage Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 239000006069 physical mixture Substances 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
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- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
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- 239000006228 supernatant Substances 0.000 description 2
- GUOCOOQWZHQBJI-UHFFFAOYSA-N 4-oct-7-enoxy-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCCCCCCC=C GUOCOOQWZHQBJI-UHFFFAOYSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010021703 Indifference Diseases 0.000 description 1
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 230000032683 aging Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 229960002685 biotin Drugs 0.000 description 1
- 235000020958 biotin Nutrition 0.000 description 1
- 239000011616 biotin Substances 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229960000304 folic acid Drugs 0.000 description 1
- 235000019152 folic acid Nutrition 0.000 description 1
- 239000011724 folic acid Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 235000021056 liquid food Nutrition 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001304 sample melting Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 238000012932 thermodynamic analysis Methods 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 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
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/40—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
-
- 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
Abstract
The invention discloses a kind of lycopene nanometer powders and preparation method thereof, the powder is that lycopene nanoemulsions are made by spray drying process, the inlet air temperature of the preparation is 170~210 DEG C, and leaving air temp is 65~105 DEG C, and feed rate is 10~30 mL/min.The method of the invention is easy to operate, the lycopene nanometer powder being prepared, storage is after one month under conditions of room temperature is protected from light dry, the load factor of lycopene is still up to 60% in nanometer powder, retention rate can be higher than 80%, average grain diameter increasing degree is 165 nm, storage stability is high, nutrient content is high, ion stability and THE STABILITY are high, illustrate that lycopene nanometer dried powder constructed by this method has the potentiality applied in food system, suits large area to popularize and apply.
Description
Technical field
The invention belongs to functional nutrient food preparation processes technical fields.It is received more particularly, to a kind of lycopene
Rice flour end and preparation method thereof.
Background technique
Lycopene (lycopene) is one kind of carotenoid, has extensive biological activity, studies have reported that
Constantly discover and confirm that lycopene has the multiple efficacies such as cancer preventing and treating, prevention and cure of cardiovascular disease and enhancing immunocompetence, so
And the property of lycopene greatly limits its application and plays, water-insoluble and unstability are wherein most important
Two factors, which greatly limits its applications to play.
Nanoemulsions are a kind of thermally labile system of partial size within the scope of 50~200nm, have good stability, often
Transparent or semitransparent state is shown as, is suitble to the various food of addition, in beverage systems.But after all lotion be a kind of thermodynamics not
Systems stabilisation, mutually the trend of the unstable states such as separation, precipitating, aging variation can not be reversed, and the change of external environment can aggravate
The generation of this trend is unfavorable for storage, transport and the application of lotion.
Therefore, pulverulent product often is made to the processing of being dried of lotion, wherein spray drying process has very strong suitable
Answering property and economy become most-often used one of method.But the difference of the factors such as different drying temperature, drying time and oxygen
It is different, different degrees of destruction can be caused to lycopene, and seriously affect its storage stability, when lycopene is destroyed
Afterwards, other thermal sensitivity nutrients in lycopene powder, such as Vc, folic acid, biotin can lose more, reduced sugar therein
Brown stain can also occur for equal substances, cause nutritive loss.
Summary of the invention
The technical problem to be solved by the present invention is to overcome existing lycopene powder poor storage stability, nutrient content are low
Defect and deficiency, a kind of lycopene nanometer powder and preparation method thereof is provided.The method of the invention is easy to operate, preparation
Obtained lycopene nano-powder particles, storage stability is high, and ion stability and THE STABILITY are high, nutrient content
It is high.
The object of the present invention is to provide a kind of lycopene nanometer powders.
Another object of the present invention is to provide a kind of lycopene nanometer powder and preparation method thereof.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of lycopene nanometer powder, the powder are that lycopene nanoemulsions pass through spray drying
Method is made, and the inlet air temperature of the preparation is 170~210 DEG C, and leaving air temp is 65~105 DEG C, and feed rate is 10~30mL/
min。
Preferably, the inlet air temperature is 170~190 DEG C.
It is highly preferred that the inlet air temperature is 190 DEG C.
Preferably, the leaving air temp is 75~95 DEG C.
It is highly preferred that the leaving air temp is 85 DEG C.
Preferably, the feed rate is 15~25mL/min.
It is highly preferred that the feed rate is 20mL/min.
Most preferably, a kind of preparation method of lycopene nanometer powder, the powder are made by spray drying process,
The inlet air temperature of the preparation is 190 DEG C, and leaving air temp is 85 DEG C, feed rate 20mL/min.
In addition, the lycopene nanometer powder obtained by above-mentioned preparation method, also within that scope of the present invention.
The invention has the following advantages:
The method of the invention is easy to operate, and the lycopene nanometer powder being prepared is protected from light dry item in room temperature
After storing one month under part, the load factor of lycopene is still up to 60% in nanometer powder, and retention rate can be higher than 80%, averagely
Partial size amplification is 165nm, and storage stability is high；Nutrient content is high；The shape of powder particle is prepared close to spherical shape, without obvious
Crack or hole；Lycopene nano particle is that 3~6 stability inferiors are preferable in pH, and ion stability and THE STABILITY are high.It says
Bright constructed nanometer dried powder has the potentiality applied in food system, suits large area to popularize and applies.
Detailed description of the invention
Fig. 1 is the original lotion of lycopene and the grain size distribution for being spray-dried lycopene powder reconstituted milk.
Fig. 2 is spray drying lycopene nanoemulsions powder reconstitution cream dilution photo.
Fig. 3 compares for the reducing power and DPPH free radical quenching activity of pure lycopene and lycopene nanometer powder.
Fig. 4 is the outside drawing and SEM figure of lycopene powder particle.
Fig. 5 is lycopene crystal powder, lycopene nano-powder particles, OSA converted starch-lycopene mixture
With the differential scanning calorimetry spectrogram of OSA converted starch.
Fig. 6 is the infared spectrum of OSA converted starch, lycopene powder particle and pure lycopene crystal.
Fig. 7 is the partial size and potential value of reconstituted milk under different NaCl concentrations.
Fig. 8 is different MgCl2The partial size and current potential of reconstituted milk under concentration.
Fig. 9 is influence of the different sucrose to nano-emulsion particle diameter and light absorption value.
Specific embodiment
The present invention is further illustrated below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
It limits in any form.Unless stated otherwise, the present invention uses reagent, method and apparatus routinely try for the art
Agent, method and apparatus.
Unless stated otherwise, following embodiment agents useful for same and material are commercially available.
A kind of preparation of the lycopene nanoemulsions of embodiment 1
A kind of load lycopene nanoemulsions, are made of oil-phase solution and aqueous phase solution, and grease phase mass ratio is 1:11,
The oil is mutually made of MCT (medium chain triglyceride) and lycopene, and the water phase is made of converted starch and deionized water, tool
Steps are as follows for body:
1, configuration quality concentration be 20~30% converted starch solution, the stirring and dissolving at 30~70 DEG C, then put to
It is stirred at room temperature, makes its abundant aquation, as water phase；
2, the lycopene oil that configuration quality concentration is 0.1~0.5%, ultrasonic dissolution under room temperature, after its dissolution completely
Filtering, as oily phase；
3, it is mutually mixed oily with water phase 1:11 in mass ratio, and the stirring and emulsifying at 50 DEG C；
4, it obtains finally loading lycopene nanoemulsions for homogeneous 3 times at 110Mpa after mixed liquor high speed dispersion.
The optimization of 2 inlet air temperature of embodiment
1, experimental procedure
Lycopene nanoemulsions are prepared with spray drying process in lycopene nanoemulsions prepared by embodiment 1
Powder.Spray drying use Shanghai Zi Yu Biotechnology Co., Ltd ZY-8000 low temperature spray drying device, hothouse having a size ofAnd it is equipped with 0.7mm bore two-fluid spray nozzle；
The operating condition of spray drying are as follows: the inlet air temperature of preparation is 170~210 DEG C, and leaving air temp is 85 DEG C, charging speed
Rate is 20mL/min.
2, experimental result
The load factor of lycopene in lycopene nanoemulsions powder is measured, the results are shown in Table 1.
The different inlet air temperature of table 1 prepare the load factor of lycopene in lycopene nanoemulsions powder
As a result, it has been found that when inlet air temperature is 170~190 DEG C, tomato red in the lycopene nanoemulsions powder of preparation
The load factor of element is higher, and effect is preferable.
The optimization of 3 leaving air temp of embodiment
1, experimental procedure
The inlet air temperature of preparation is 190 DEG C, and leaving air temp is 65~105 DEG C, feed rate 20mL/min, other preparations
Conditioned reference embodiment 2.
2, experimental result
The load factor of lycopene in lycopene nanoemulsions powder is measured, the results are shown in Table 2.
The different leaving air temps of table 2 prepare the load factor of lycopene in lycopene nanoemulsions powder
As a result, it has been found that when leaving air temp is 75~95 DEG C, lycopene in the lycopene nanoemulsions powder of preparation
Load factor it is higher, effect is preferable.
The optimization of 4 feed rate of embodiment
1, experimental procedure
The inlet air temperature of preparation is 190 DEG C, and leaving air temp is 85 DEG C, and feed rate is 10~30mL/min, other preparations
Conditioned reference embodiment 2.
2, experimental result
The load factor of lycopene in lycopene nanoemulsions powder is measured, the results are shown in Table 3.
The different leaving air temps of table 3 prepare the load factor of lycopene in lycopene nanoemulsions powder
As a result, it has been found that when feed rate is 15~25mL/min, tomato in the lycopene nanoemulsions powder of preparation
The load factor of red pigment is higher, and effect is preferable.
A kind of preparation method of the lycopene nanoemulsions powder of embodiment 5
1, experimental procedure
The inlet air temperature of preparation is 190 DEG C, and leaving air temp is 85 DEG C, feed rate 20mL/min, other preparation conditions
Reference implementation example 2 is measured the load factor of lycopene in lycopene nanoemulsions powder.
2, experimental result
Work as preparation condition: inlet air temperature is 190 DEG C, and leaving air temp is 85 DEG C, when feed rate is 20mL/min, preparation
The load factor of lycopene is up to 79.36% in lycopene nanoemulsions powder.
6 orthogonal optimization of embodiment
1, experimental procedure
According to single factor experiment as a result, inlet air temperature is selected to be 75~95 DEG C for 170~190 DEG C, leaving air temp and feed
Rate is 15~25mL/min, this 3 factors are as orthogonal investigation factor, using the design of Three factors-levels, with load factor
For response and interpretation of result is carried out, other preparation condition reference implementation examples 2.
4 orthogonal test factor of table and water-glass
2, experimental result
The results are shown in Table 5 for orthogonal optimization test.
5 orthogonal experiments of table (n=9)
2, experimental result
As shown in Table 5, the load factor highest of the 8th group of lycopene, it is identical with single factor test optimum results up to 79.36%,
I.e. when inlet air temperature is 190 DEG C, leaving air temp is 85 DEG C, and when feed rate is 20mL/min, load factor highest is 79.36%.
The stability study of 7 lycopene nano-powder particles of embodiment
1, experimental procedure
1.1, by lycopene powder particle is prepared under different condition in table 6, store 30 days under conditions of room temperature is protected from light,
Select raw material tomato red pigment nanoemulsions as a control group；
1.2 configuration reconstituted milks: lycopene powder particle is prepared in table 6 under different condition, powder and deionized water are pressed
It is configured according to 5:6；
1.3 take 1mL deionized water to redissolve the powder after 0.2g storage, and with magnetic stirrer until uniform, to kind
The content of Lycopene is measured, and calculates its load factor and retention rate, is measured to the partial size of lycopene powder particle, kind
Lycopene solution meets Lambert-Beer's law in the low concentration range, therefore selects the amount of spectrophotometry measurement lycopene,
Specific assay method is as follows:
1.3.1 Specification Curve of Increasing: accurately weighing 2.1mg lycopene mark product, with the dissolution of a small amount of methylene chloride, is added just
It is No. 1 mother liquor that hexane, which is settled to 10mL,.Distribution draws 10,50,100,500,1000,2000 μ L and is placed in 6 in No. 1 mother liquor
In the volumetric flask of 10mL, n-hexane is added to shake up to scale, that is, be made into lycopene mass concentration be 0.2,1.0,5.0,10.0,
20.0, the standard solution of 40.0 μ g/mL.Using n-hexane as reference, its absorbance is successively surveyed at 472nm；
1.3.2 lycopene content measure: take 200 μ L lycopene samples uniformly to mix with the DMSO of 800 μ L, then according to
The secondary n-hexane that 2mL is added: the mixing organic phase (3:1, v:v) of methylene chloride is extracted, and merges extraction after repeating extraction 3 times
Liquid is centrifuged 10min at 3,000 rpm, and supernatant liquor is taken to be placed under spectrophotometer the light absorption value for measuring lycopene.With just oneself
For alkane as blank control, measurement wavelength is 472nm, is as a result calculated by standard curve.
1.3.3 the load factor of lycopene
Shown in accounting equation such as formula (2.1):
In formula, C1After -30 days in powder lycopene content；C0The content of lycopene in the preceding lotion of-storage.
1.3.4 the retention rate of lycopene
Shown in accounting equation such as formula (2.2):
In formula, C2- after storage time 30 days in powder lycopene content；C3- store lycopene in preceding powder
Content.
1.3.5 particle size determination
Using nano particle size and Zeta potential analyzer Zetasizer Nano ZS90 (equipped with He/Ne laser (λ=
633nm)) measure the partial size of lotion.100 times first are diluted to reconstituted milk using deionized water before all samples test, is then drawn
The prepare liquid of (about the 1/3 of cuvette) is added in quartz colorimetric utensil in right amount, and 2~3min, each sample are kept the temperature at 25 ± 0.1 DEG C
Product are repeated three times.
The preparation of lycopene powder particle under 6 different condition of table
2, experimental result
The measurement result of retention rate and load factor to lycopene powder grain diameter and its lycopene such as 7 institute of table
Show.
The measurement knot of the retention rate and load factor of lycopene powder grain diameter and its lycopene after table 7 is stored 30 days
Fruit
As shown in Table 7, under optimum preparating condition, lycopene powder particle is stored 30 days under conditions of room temperature is protected from light
Afterwards, the load factor of lycopene is up to 60.42%, and retention rate is up to 81.24%, and its partial size hardly happens variation, and
The load factor of lycopene and retention rate also respectively reach 40% in the lycopene powder particle prepared under other different conditions
With 69% or more, storage stability is much higher than control group, illustrates that this technique can greatly improve the guarantor of lycopene powder particle
The time is hidden, it is to improve shelf stability and ease of use one effectively way that powder, which is made, in nanoemulsions with spray drying process
Diameter.
The dissolution characteristics and its partial size of 8 lycopene nanometer powder of embodiment are studied
1, the water of lycopene nanometer powder redissolves Journal of Sex Research
1.1 experimental procedure
In order to investigate the water solubility of spray drying lycopene powder, 1mL deionized water is specially taken to redissolve 0.2g dry
Powder after dry, and with magnetic stirrer until uniformly, visually observing its mode of appearance.
1.2 experimental result
As a result powder particle shows good rehydration dissolubility, caking phenomenon does not occur, and system is uniformly dissolved.
2, the partial size research of lycopene nanometer powder
2.1 experimental procedure
It is surveyed using partial size and particle diameter distribution of the Malvern Particle Size Analyzer to the original lotion of lycopene and reconstituted milk
Fixed, specific measuring method is referring to [embodiment 7].
Using nano particle size and Zeta potential analyzer ZetasizerNano ZS90 (equipped with He/Ne laser (λ=
633nm)) measure the coefficient of dispersion (Poly dispersity Index, PDI) of former lotion and reconstituted milk, remaining step referring to
[embodiment 7].
2.2 experimental result
As a result as shown in Figure 1.As seen from the figure, original emulsion and the particle diameter distribution difference of reconstituted milk are not obvious, and two
Person shows as relatively narrow unimodal shape, and the original lotion of lycopene and the average grain diameter of reconstituted milk be respectively 150nm and
151nm, for partial size without significant change, PDI is respectively less than 0.25, and centralized particle diameter illustrates that lycopene prepared by the present invention is received
Rice flour end and original emulsion partial size indifference.
It further illustrates, spray drying process of the present invention will not influence the dissolution characteristics of lycopene nanoemulsions
And particle size, the reasonability to use spray drying process to prepare nanoemulsions powder-product provide certain data support.
Uniformity research after the standing of 9 lycopene nanometer powder of embodiment
1, uniformity research after the standing of lycopene nanometer powder
1.1 experimental procedure
1.1.1 reconstituted milk is prepared, specific preparation method is referring to [embodiment 7]；
1.1.2 the reconstituted milk of lycopene powder particle is diluted after being stood for 24 hours after 1,2 and 3 times, observes its shape
State.
1.2 experimental result
As a result as shown in Fig. 2, after standing for 24 hours after reconstituted milk to be diluted to 1,2 and 3 times respectively, reconstituted milk still keeps good
The uniformity.Illustrate that nanometer powder redissolution rear stability is still good, drying process will not influence the performance of lotion itself.
The chemical antioxidant activity research of 10 lycopene nanometer powder of embodiment
In order to investigate spray-drying process high temperature condition to the damage influence degree of lycopene in powder particle, design
Its chemical antioxidant activity is studied in experiment.
1, experimental procedure
The measurement of 1.1 reducing powers
1.1.1 it weighs a certain amount of lycopene powder sample and is dissolved in phosphate buffer and reconstituted milk is made；
1.1.2 it mixes the reconstituted milk of 1mL and the 1mL potassium ferricyanide (1%, w/v) is placed in the heating water bath at 50 DEG C
20min；
1.1.3 1mL trichloroacetic acid (10%, w/v) is added, it is complete to solution reaction；
1.1.4 it is centrifuged 20 minutes under 3000rpm revolving speed, the iron chloride of 0.5mL 20mM/L is added after supernatant is removed
Solution 1mL deionized water, surveys its light absorption value under 700nm wavelength after mixing evenly, and control group is to be dissolved in tetrahydrofuran/diformazan Asia
The water solution of lycopene of sulfone (1:1, v/v).
The measurement of 1.2 scavenging ability of DPPH free radical
1.2.1 the preparation of reconstituted milk；
1.2.2 taking three test tubes to define test tube A1 respectively is sample, and test tube A2 is reference, and test tube A3 is blank, is added by table 8
Enter reagent, wherein sample sets water-bath 30min at 25 DEG C；
1.2.3 the measurement of absorbance is carried out, at 517nm respectively with the zeroing of 95% ethanol solution.Control group is to be dissolved in four
Hydrogen furans/dimethyl sulfoxide (1:1, v/v) water solution of lycopene.
Table 8 eliminates DPPH free radical and is loaded table
Sample can be formulated as Scavenging activity, that is, clearance rate of DPPH free radical:
DPPH clearance rate (%)=[1- (A1-A3)/A2] × 100
2, experimental result
As a result if Fig. 3 is (shown in a, as can be seen from Figure, along with the increase of lycopene concentration, the reducing power of sample
Enhance, under same concentration, the reducing power of lycopene nano-powder particles is intended to much higher than free lycopene crystal.
As a result as (consistent with reducing power variation tendency shown in b, the DPPH free radical quenching ability of sample is with tomato by Fig. 3
The increase of lycopene concentration and increase, and under the conditions of same concentrations, the quenching ability of lycopene nano-powder particles compares tomato
Red pigment is slightly larger.
As a result illustrate that the chemical characteristic for the lycopene nano-powder particles to be formed compared with free lycopene, restores
Power and higher to the quenching ability of DPPH free radical, illustrates hot conditions of this method in spray-drying process not to powder
Lycopene causes to damage in particle.
The morphosis of 11 lycopene nano-powder particles of embodiment is studied
1, experimental procedure
1.1 observe lycopene nano-powder particles using naked eyes；
1.2 reference implementation examples 7 prepare reconstituted milk, are diluted and 100 times and are shaken up with deionized water, after being dipped with glass bar point in
On glass slide, covered carries out mode of appearance observation with SEM and takes pictures, and amplification factor is 1000 times.
2, experimental result
As a result as shown in figure 4, as can be seen from Figure, lycopene nano-powder particles color and dispersion degree are uniform, do not have
The phenomenon that occurring agglomeration illustrates that spray drying condition works well.It is from SEM micrograph piece it is also seen that bright between particle
Aobvious separation, does not stick together.Further illustrate that the application records spray drying condition and works well.
The thermodynamic behaviour of 12 lycopene nano-powder particles of embodiment
1, the thermodynamic analysis of lycopene nano-powder particles
1.1 experimental procedure
Utilize differential scanning calorimetry lycopene nano-powder particles, lycopene crystal, lycopene-OSA
The thermodynamic behaviour of converted starch (starch octenylsuccinate) physical mixture and OSA converted starch, specific steps are such as
Under:
The HDSCPT500LT/1400 low temperature that differential scanning thermometric analysis instrument is produced using Lin Saisi Linseis company, Germany
Differential scanning calorimetric analysis instrument configures liquid nitrogen cryogenics controller；
Instrument is corrected using preceding with indium, and 1h is balanced at 109 DEG C, and it is 10 that setting temperature condition, which is heating rate,
DEG C/min, temperature range is 50~300 DEG C, test sample thermodynamic parameter；
Using empty rustless steel container as control in experiment, the weight of the nano-powder particles in each stainless steel sample container
Amount should be less than 10mg, and be sealed with the stainless steel lid containing O-type plastic hoop, be then placed on corresponding position；
Software is carried with instrument data are analyzed to obtain sample melting enthalpy and crystalline melt temperatures, each sample weight
Again three times.
1.2 experimental result
Lycopene nano-powder particles, lycopene crystal, lycopene-OSA converted starch physical mixture and OSA
The differential scanning amount result of converted starch is as shown in Figure 5.As a result, it has been found that in the range of 50~300 DEG C, lycopene nano powder
Last particle does not have to find the melting peakss of lycopene in detection range, illustrates the lycopene in nanometer powder with water solubility more
High amorphous state exists.
Further illustrate that the lycopene nano-powder particles dissolubility of this method preparation is more preferable, the lycopene of embedding is molten
Solution property is also improved, and is conducive to the following addition in beverage, liquid food system, is convenient for absorption of human body.
2, the structural analysis of lycopene nano-powder particles
2.1 experimental procedure
It is brilliant to detect lycopene powder particle, OSA converted starch and lycopene respectively using Fourier infrared spectrograph
Body passes through the change of the variation mapping structure of matter of abosrption spectrogram, the specific steps are as follows:
2.1.1 the test of sample use pellet technique, weigh respectively the appropriate lycopene of 1mg, OSA converted starch,
Lycopene nanoemulsions powder sample is sufficiently mixed with 100mg potassium bromide；
2.1.2 it is ground under the irradiation of infrared lamp, ground mix powder is poured on template later, be perfused
Pressing mold is pressed into transparent sheet-like with tablet press machine；
2.1.3 thin slice is taken out, is placed in infrared spectrograph sample room, in 400~4000cm-1It is scanned in range, light
Spectral resolution is 4cm-1；
2.1.4 it uses air for blank in experiment, obtains the infrared spectrogram of sample after scanning signal is 16 times cumulative.
2.2 experimental result
Infrared analysis result such as Fig. 6 institute of lycopene nano-powder particles, OSA converted starch and lycopene crystal
Show, as seen from the figure, lycopene crystal is in wavelength 959cm-1Locate strong trans- characteristic peak to be blanked, shows lycopene by starch point
Sub- emulsion layer embedding is complete.After embedding, OSA converted starch is in 2930cm-1Methyl stretching vibration peak shift to 2927cm-1, and
2856cm-1Located newly-generated one vibrate this may be related to the loading of lycopene, can speculate starch molecule and lycopene
Between there may be interaction of hydrogen bond.In addition, lycopene nanoemulsions powder is in 1745cm-1It has been formed about strong suction
Peak is received, is herein the stretching vibration of typical C=O, the ester bond in oily phase is represented in the powder systems, further illustrates this
The lycopene nano-powder particles of invention preparation do not destroy the structures of lycopene nanoemulsions, oil mutually and starch molecule it
Between still well combine, it is with good stability compared to OSA converted starch and lycopene crystal.
13 lycopene nano-powder particles of embodiment apply stability study
1, pH Stability Determination
1.1 experimental procedure
The stability of lycopene nanometer powder under different pH environment is studied, and to its partial size, PDI, Zeta electricity
Position and light absorption value are measured, the specific steps are as follows:
1.1.1 suitable lycopene nanometer powder is taken, it is slow to be dissolved in the phosphate that pH is 2,3,4,5,6,7,8 and 9 respectively
In fliud flushing, 100 times are diluted with corresponding buffer and is placed on equilibrium at room temperature 4h.
1.1.2 its partial size and PDI value are measured, referring specifically to [embodiment 7], and measures its light absorption value at 600nm.
1.1.3Zeta potential measurement: sample container is used polystyrene cuvette instead and is tested.The pre-processing of sample and
Other determination steps are referring specifically to [embodiment 7].
1.1.4PDI measure: specific method is referring to [embodiment 8].
1.2 experimental result
The stability of lycopene nanometer powder under different pH environment is studied, the results are shown in Table 9.
Average grain diameter, PDI, Zeta potential and the light absorption value of nanoemulsions under 9 difference pH of table
As shown in Table 9, the Zeta potential value of lycopene reconstituted milk is incremented by, particle diameter with the rising of pH, PDI and
The changing rule for first reducing and increasing afterwards is then presented in light absorption value, it is possible thereby to find, peracid or alkali excessively can all seriously affect sample
Performance.
Generally, lycopene nano particle is relatively stable in the range of pH is 3~6, and electrostatic repulsion subtracts at this time
Weak but powerful steric hindrance effect ensure that the stability of nano particle diameter.
2, ion stability measures
2.1 experimental procedure
2.1.1 the MgCl that the NaCl solution and concentration that configuration concentration is 0~1mol/L are 0~0.016mol/L2Solution；
2.1.2 lycopene nanometer powder is redissolved with the salt ion solution of various concentration, 100 times of dilution is placed on
Equilibrium at room temperature 4h；
2.1.3 measurement reconstituted milk partial size specific method is referring to [embodiment 7].
2.1.4 Zeta potential value is measured, specific method is referring to above-mentioned pH Stability Determination step 1.1.3.
2.2 experimental result
The addition of electrolyte can reduce Zeta potential, this is because being to pass through with the stable nanoemulsions of OSA converted starch
The electrostatic repulsion and steric hindrance of oil-water interfaces layer act on the stabilization to maintain particle, are attached to after electrolyte ion addition
Oil-water interfaces layer, compression boundary layer keep its thinning, reduce potential value；Meanwhile negatively charged R-COO?Generated electrostatic row
Reprimand is acted on because by Na+And Mg2+It shields and weakens, softened molecular structure, the space model that individual molecule is occupied in oil-water interfaces
Diminution is enclosed, more OSA Molecular Adsorptions enhance in particle surface, the space steric effect of system, can effectively slow down particle aggregation.
As a result as shown in Figure 7 and Figure 8.It can be seen from the figure that Na+And Mg2+Addition can lead to the Zeta potential of particle
It is remarkably decreased, however the NaCl of various concentration and MgCl2The partial size of nano particle can't be significantly affected, the partial size of the two increases
Amplitude is no more than 10%.Illustrate having good stability for lycopene nanometer powder, the salt ion in food system has no effect on
Its service performance is conducive to for lycopene nano-powder particles being added in food system.
3, THE STABILITY measures
3.1 experimental procedure
3.1.1 the sucrose solution of configuration quality concentration 2~18%；
3.1.2 lycopene nanometer powder is redissolved with the sucrose solution of above-mentioned mass concentration, dilutes 100 times of postpositions
In equilibrium at room temperature 4h；
3.1.3 its partial size is measured, referring specifically to [embodiment 7], and measures its light absorption value at 600nm.
3.2 experimental result
As a result as shown in figure 9, it can be seen from the figure that when sucrose concentration rises to 18% from 2%, nanometer in system
The partial size of grain increases to 228nm by 151nm, and increasing degree reaches 50%, illustrates sucrose concentration to lycopene nanometer powder
The grain diameter influence of grain is significant.And along with the increase of concentration, light absorption value becomes smaller, and the appearance of sample becomes more transparent.
In conclusion the concentration of sucrose not only will not influence the stability of lycopene nano particle in food and drink, also
Be conducive to improve its application effect.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of lycopene nanometer powder, which is characterized in that the powder is that lycopene nanoemulsions are logical
It crosses spray drying process to be made, the inlet air temperature of the preparation is 170~210 DEG C, and leaving air temp is 65~105 DEG C, feed rate
For 10~30 mL/min.
2. method according to claim 1, which is characterized in that the inlet air temperature is 170~190 DEG C.
3. method according to claim 1, which is characterized in that the inlet air temperature is 190 DEG C.
4. method according to claim 1, which is characterized in that the leaving air temp is 75~95 DEG C.
5. method according to claim 1, which is characterized in that the leaving air temp is 85 DEG C.
6. method according to claim 1, which is characterized in that the feed rate is 15~25 mL/min.
7. method according to claim 1, which is characterized in that the feed rate is 20 mL/min.
8. the lycopene nanometer powder being prepared by any the method for claim 1~7.
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