CN106993741A - A kind of method for improving leaf of bamboo antioxidant stability - Google Patents
A kind of method for improving leaf of bamboo antioxidant stability Download PDFInfo
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- CN106993741A CN106993741A CN201710127761.7A CN201710127761A CN106993741A CN 106993741 A CN106993741 A CN 106993741A CN 201710127761 A CN201710127761 A CN 201710127761A CN 106993741 A CN106993741 A CN 106993741A
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- leaf
- bamboo
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- bamboo antioxidant
- cyclodextrin
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- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 106
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 106
- 241001330002 Bambuseae Species 0.000 title claims abstract description 106
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 106
- 239000011425 bamboo Substances 0.000 title claims abstract description 106
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 99
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 56
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 150000001875 compounds Chemical class 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 5
- 235000006708 antioxidants Nutrition 0.000 claims description 85
- 229930003944 flavone Natural products 0.000 claims description 23
- 235000011949 flavones Nutrition 0.000 claims description 23
- 239000003643 water by type Substances 0.000 claims description 14
- 150000002213 flavones Chemical class 0.000 claims description 8
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 8
- 229920000053 polysorbate 80 Polymers 0.000 claims description 8
- NWGKJDSIEKMTRX-MDZDMXLPSA-N Sorbitan oleate Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(O)C1OCC(O)C1O NWGKJDSIEKMTRX-MDZDMXLPSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 18
- 238000012360 testing method Methods 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 230000007760 free radical scavenging Effects 0.000 abstract description 2
- 244000010375 Talinum crassifolium Species 0.000 abstract 1
- 235000015055 Talinum crassifolium Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 150000003254 radicals Chemical class 0.000 description 22
- 239000007864 aqueous solution Substances 0.000 description 19
- 235000019441 ethanol Nutrition 0.000 description 16
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 14
- 150000002212 flavone derivatives Chemical class 0.000 description 14
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 14
- 238000002835 absorbance Methods 0.000 description 12
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 10
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 10
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 10
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 10
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 10
- 235000005493 rutin Nutrition 0.000 description 10
- 229960004555 rutoside Drugs 0.000 description 10
- 239000000523 sample Substances 0.000 description 7
- 238000002798 spectrophotometry method Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 235000013305 food Nutrition 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 210000003298 dental enamel Anatomy 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920000136 polysorbate Polymers 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 235000019261 food antioxidant Nutrition 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- 244000000231 Sesamum indicum Species 0.000 description 1
- 235000003434 Sesamum indicum Nutrition 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- -1 compound Flavones Chemical class 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
- 238000005406 washing 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- 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
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Botany (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of method for improving leaf of bamboo antioxidant stability, methods described is：Leaf of bamboo antioxidant is dissolved in ethanol water leaf of bamboo antioxidant solution is made；Cyclodextrin is mixed with emulsifying agent is added after deionized water dissolving, cyclodextrin solution is made again；Cyclodextrin solution is heated to 30 60 DEG C, the 60min of stirring reaction 30 after leaf of bamboo antioxidant solution, completion of dropping is slowly added dropwise, reaction solution vacuum distillation is removed and dried after ethanol, leaf of bamboo antioxidant cyclodextrin inclusion compound is obtained, the raising of leaf of bamboo antioxidant stability is realized；The leaf of bamboo antioxidant cyclodextrin inclusion compound that the present invention is developed, is significantly improved compared with raw material on antioxidative stabilizer, improves more than 1 times.By 60 DEG C of accelerated oxidation test, after 30 days, the free radical scavenging activity of raw material does not reach the half of inclusion compound, absolutely proves that inclusion compound plays the role of good holding leaf of bamboo antioxidant properties, improves water solubility, improve its application performance.
Description
(1) technical field
The present invention relates to a kind of method for improving leaf of bamboo antioxidant stability.
(2) background technology
Leaf of bamboo antioxidant has been approved as food additives China is relatively early, its basis be bamboo-leaves flavones, lactone and
Phenolic acid.It can be widely applied to numerous food anti-oxidant, have the advantages that source is natural, safe.But leaf of bamboo antioxidant exists
Stability is still not high enough in storage process, has itself certain oxidized phenomenon, influences its application value.Current manufacturing enterprise adopts
Reduced and itself in leaf of bamboo antioxidant storage process be oxidized with methods such as vacuum packaging, lucifuge storages, but effect is not
Ideal, thus, the stability of leaf of bamboo antioxidant itself is improved, it is preferably applied in food processing, it is significant.
(3) content of the invention
It is an object of the present invention to provide a kind of method for improving leaf of bamboo antioxidant stability, ring is made in leaf of bamboo antioxidant
Cyclodextrin inclusion compound, reduces leaf of bamboo antioxidant itself and is oxidized, improve it as the stability of food additives, change while having
The effect of kind leaf of bamboo antioxidant local flavor, enables leaf of bamboo antioxidant to be preferably applied to food.
The technical solution adopted by the present invention is：
The present invention provides a kind of method for improving leaf of bamboo antioxidant stability, and methods described is：By leaf of bamboo antioxidant
It is dissolved in volumetric concentration 30-50% ethanol waters and leaf of bamboo antioxidant solution is made；Again by cyclodextrin deionized water dissolving
After add emulsifying agent, mix, cyclodextrin solution is made；Cyclodextrin solution is heated to 30-60 DEG C, the leaf of bamboo is slowly added dropwise anti-oxidant
Stirring reaction 30-60min after agent solution, completion of dropping, reaction solution vacuum distillation is removed and dried after ethanol, obtains the leaf of bamboo anti-oxidant
Agent cyclodextrin inclusion compound, realizes the raising of leaf of bamboo antioxidant stability；The emulsifying agent is Tween 80 or sorbester p17；The bamboo
Leaf antioxidant is 1 with cyclodextrin, emulsifying agent mass ratio:1-10：0.001-0.1；The ethanol water volumetric usage is with bamboo
Leaf antioxidant quality is calculated as 20-40L/kg, and the deionized water volumetric usage is calculated as 20-50L/kg with cyclodextrin quality.
Further, flavones mass content is 25-40% in the leaf of bamboo antioxidant, and the leaf of bamboo antioxidant is the leaf of bamboo
Extract, as food antioxidant, preferably purchased from Hangzhou Zhong Zhikang mushrooms Bioisystech Co., Ltd.
Further, the ethanol water volumetric usage is preferably 20L/kg in terms of leaf of bamboo antioxidant quality.
Further, the deionized water volumetric usage preferred 25L/Kg in terms of cyclodextrin quality.
Further, the leaf of bamboo antioxidant solution rate of addition is 1L/min.
Further, the reaction solution is evaporated in vacuo to spray at 120-150 DEG C after removal ethanol at 0.1Pa, 60 DEG C and done
It is dry.
Further, the leaf of bamboo antioxidant and cyclodextrin, emulsifying agent mass ratio are 1:4-7：0.002-0.005.
Compared with prior art, beneficial effect of the present invention is mainly reflected in：
The leaf of bamboo antioxidant cyclodextrin inclusion compound that the present invention is developed, has compared with raw material on antioxidative stabilizer and substantially carries
Height, is improved more than 1 times.By 60 DEG C of accelerated oxidation test, after 30 days, the free radical scavenging activity of raw material does not reach the one of inclusion compound
Half, absolutely prove that inclusion compound there are good holding leaf of bamboo antioxidant properties.Meanwhile, leaf of bamboo antioxidant is by the present invention
Method after cyclodextrin encapsulated, to improve water solubility, can be completely dissolved in pure water, the aqueous solution can reach no leaf of bamboo taste, carry
Its application performance is risen.
(4) embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment 1：
(1) weighing 1000 grams of leaf of bamboo antioxidant, (its general flavone mass content of spectrophotometry is 30%, purchased from west
The bright bio tech ltd in Anze), it is dissolved in 20 liters of ethanol waters of volumetric concentration 40%, stirring makes it fully dissolve,
Leaf of bamboo antioxidant solution is made.6000 grams of food-grade cyclodextrin (being purchased from Zibo Qian Hui bio tech ltd) are weighed, it is molten
Solution is in 150 liters of deionized waters, then weighs 4.0 grams of food grade emulsifier tweens 80, is dissolved in cyclodextrin aqueous solution, in enamel still
In stir, form the cyclodextrin Tween 80 aqueous solution, and be heated to 40 DEG C, resist the leaf of bamboo in being stirred continuously under constant temperature
Oxidizing agent solution is slowly added into the cyclodextrin Tween 80 aqueous solution, per minute to add 1 liter or so, total 20 minutes time of addition.
Mixing is added to finish, then keeping temperature continues to stir 50 minutes.Stirring is finished under 0.1 atmospheric pressure vacuum, 60 DEG C of vacuum are steamed
Recovery ethanol is evaporated, recovery is finished, be spray-dried with 140 DEG C of hot blast temperature, obtain leaf of bamboo antioxidant cyclodextrin inclusion compound
6716g。
(2) measure of the general flavone in leaf of bamboo antioxidant
Using rutin as standard items, using the general flavone in spectrophotometry leaf of bamboo antioxidant, with the bag of general flavone
Conjunction rate characterizes cyclodextrin encapsulated effect.Detection method is as follows：
1) standard curve：Rutin standard items, purity 98.5%, are purchased from Nat'l Pharmaceutical ＆ Biological Products Control Institute.Rutin standard
Solution is prepared：Rutin standard items 11.6mg accurately is weighed, the ethanol water dissolving and constant volume with volumetric concentration 60% are in 50mL
In volumetric flask, concentration is obtained for 0.232mgmL-1Rutin standard liquid.
Take rutin standard liquid 2.0,3.0,4.0,5.0,6.0,7.0,8.0mL respectively with pipette, be respectively placed in 25mL
In volumetric flask, plus the ethanol water of volumetric concentration 60% is supplemented to 10mL, respectively toward the mass concentration of addition 0.7mL in each bottle
5% sodium nitrite in aqueous solution, shakes up placement 5min, then adds the 0.7mL aluminum nitrate aqueous solution of mass concentration 10%, shake up and put
5min is put, the 5ml sodium hydrate aqueous solution of mass concentration 4.3% is added, placement 5min is shaken up, finally with volumetric concentration 60%
Ethanol water constant volume is put at 25mL graduation marks, is shaken up.Its absorbance is surveyed at 510nm with ultraviolet specrophotometer, with not
Plus rutin standard liquid is blank control.With rutin concentration C (mgmL-1) it is ordinate, measured absorbance (A) is horizontal stroke
Coordinate, draws standard curve, obtains the concentration C (mgmL of rutin-1) be with the regression equations of absorbance A standard curves：C
=0.0935A-0.0011, R2=0.9996, as a result show, the concentration of absorbance and rutin is in good linear relationship.
2) detection of sample general flavone：Take 0.05g samples, with the dissolving of the ethanol water of volumetric concentration 60% and constant volume in
In 50mL volumetric flask, take 5.0ml to be placed in 25mL volumetric flasks with pipette, existed according to the assay method of above standard curve
Its absorbance is surveyed at 510nm, according to the absorbance measured and according to the concentration of flavones in regression equation calculation sample.
(3) measure of leaf of bamboo antioxidant cyclodextrin inclusion compound general flavone inclusion rate：
The assay of inclusion compound surface flavones：It is accurate to weigh 0.6g leaf of bamboo antioxidant inclusion compound products, add 20mL
After absolute ethyl alcohol, fully vibration, washing, it is transferred in 50mL volumetric flasks, then uses absolute ethyl alcohol constant volume, stand, filtering takes
2mL filtrates calculate the content of inclusion compound surface flavones by the absorbance that rutin is standard items spectrophotometry filtrate.
The measure of inclusion compound product flavones total amount：0.6g leaf of bamboo antioxidant cyclodextrin inclusion compound products accurately are weighed, plus
After 20mL distilled water is dissolved by heating, it is transferred in 50mL volumetric flasks, then uses absolute ethyl alcohol constant volume, is fully vibrated through ultrasound quiet
Put, filter, take 1mL filtrates by the absorbance that rutin is standard items spectrophotometry filtrate, calculate inclusion compound general flavone
Content.
The inclusion rate of inclusion compound is calculated as follows:
A (%)=(1-B/C) × 100%
In formula, A is the inclusion rate (%) of inclusion compound；B is the flavones quality (mg) on inclusion compound surface；C is total in inclusion compound
Flavones quality (mg).
(4) stability of leaf of bamboo antioxidant cyclodextrin inclusion compound, reference are detected《Pharmacopoeia of People's Republic of China》2010
Year version accelerated test method, using leaf of bamboo antioxidant raw material to compare, using Phen Fe2+It is anti-oxidant that oxidizing process determines the leaf of bamboo
The living radical clearance rate of agent inclusion compound and raw material, as the evaluation of antioxidative stabilizer, specific method is：By leaf of bamboo antioxygen
Agent powder and leaf of bamboo antioxidant cyclodextrin inclusion compound are placed in (60 ± 2) DEG C insulating box, carry out antioxidative stabilizer experiment,
A sample was taken every five days, using Phen Fe2+Oxidizing process determines its clearance rate to living radical.
Method operation is as follows：Take 0.2ml 5 × 10-3mol·L-1The Phen aqueous solution and 1ml 50mmolL- 1Tris-HCl cushioning liquid (pH=7.4 is prepared with deionization) adds 0.2ml 7.5 × 10 in 5ml volumetric flasks-3mol·
L-1FeSO4The aqueous solution, shakes up immediately, adds the sample aqueous solution that 200 μ L concentration are 10 μ g/mL, adds 0.2ml mass concentrations
L% H2O2, use ethanol constant volume.After fully shaking up, it is placed in 37 DEG C of water-baths and is incubated 60min, then existed with spectrophotometer
Its absorbance is surveyed at 536nm.Its clearance rate is calculated as follows：
N=[(A2-A3)/(A1-A3)] × 100%
In formula：N is clearance rate (%)；A1 is to be not added with H2O2Absorbance during with sample；A2 is to add H2O2During with sample
Absorbance；A3 is to add H2O2, but absorbance when being not added with sample.
After testing, general flavone inclusion rate was up to 88%, through accelerated oxidation test in 60 DEG C of insulating boxs, the 15th day for gained inclusion compound
Leaf of bamboo antioxidant cyclodextrin inclusion compound removes free radical rate and retains 93%, and raw material removes free radical rate and retains 78%, the 20th day
Leaf of bamboo antioxidant cyclodextrin inclusion compound removes free radical rate and retains 86%, and raw material removes free radical rate and retains 60%, the 30th day
Leaf of bamboo antioxidant cyclodextrin inclusion compound retains 66%, and raw material removes free radical rate and retains 31%.
Leaf of bamboo antioxidant cyclodextrin inclusion compound 1.0g is weighed, 10ml deionized waters is added, is stirred at room temperature, can be complete
It is dissolved as clear solution.Sample solution is compared, no leaf of bamboo taste through tasting with 40% ethanol solution of leaf of bamboo antioxidant.
Embodiment 2：
Weighing 1000 grams of leaf of bamboo antioxidant, (its general flavone content of spectrophotometry is 25%, purchased from many sesames in Hangzhou
Kang Gu Bioisystech Co., Ltd), it is dissolved in 40 liters of ethanol waters of volumetric concentration 30%, stirring makes it fully dissolve, makes
Into leaf of bamboo antioxidant solution.Weigh 4000 grams of food-grade cyclodextrin (purchased from sea salt six and starch Chemical Industry Co., Ltd), dissolving
In 180 liters of deionized waters, then 3.0 grams of food grade emulsifier spans 80 are weighed, be dissolved in cyclodextrin aqueous solution, in enamel still
Stir, form the cyclodextrin sorbester p17 aqueous solution, and be heated to 30 DEG C, by leaf of bamboo antioxygen in being stirred continuously under constant temperature
Agent solution is slowly added into the cyclodextrin sorbester p17 aqueous solution, per minute to add 1 liter or so, total 20 minutes time of addition.Plus
Enter mixing to finish, then keeping temperature continues to stir 30 minutes.Stirring finishes under 0.1 atmospheric pressure vacuum 60 DEG C and is evaporated in vacuo back
Ethanol is received, recovery is finished, be spray-dried with 150 DEG C of hot blast temperature, obtain leaf of bamboo antioxidant cyclodextrin inclusion compound 4702g.
Using the method for embodiment 1, after testing, general flavone inclusion rate is up to 85%, through adding in 60 DEG C of insulating boxs for gained inclusion compound
Fast oxidation test, the 15th day leaf of bamboo antioxidant inclusion compound removes free radical rate and retains 91%, and raw material is removed free radical rate and retained
79%, the 20th day leaf of bamboo antioxidant inclusion compound removes free radical rate and retains 85%, and raw material removes free radical rate reservation 61%, the
30 days leaf of bamboo antioxidant inclusion compounds retain 65%, and raw material removes free radical rate and retains 30%.
Leaf of bamboo antioxidant cyclodextrin inclusion compound 1.0g is weighed, 10ml deionized waters is added, is stirred at room temperature, can be complete
It is dissolved as clear solution.Sample solution is compared, no leaf of bamboo taste through tasting with 40% ethanol solution of leaf of bamboo antioxidant.
Embodiment 3：
Weighing 1000 grams of leaf of bamboo antioxidant, (its general flavone content of spectrophotometry is 40%, purchased from Shaanxi Bai Wei
Bio tech ltd), it is dissolved in 30 liters of ethanol waters of volumetric concentration 50%, stirring makes it fully dissolve, and bamboo is made
Leaf antioxidant solution.7000 grams of food-grade cyclodextrin (being purchased from Wuxi City Jian Xing starch-based products Co., Ltd) are weighed, are dissolved in
In 140 liters of deionized waters, then 5.0 grams of food grade emulsifier tweens 80 are weighed, be dissolved in cyclodextrin aqueous solution, filled in enamel still
Point stir, form the cyclodextrin Tween 80 aqueous solution, and be heated to 60 DEG C, it is in being stirred continuously that the leaf of bamboo is anti-oxidant under constant temperature
Agent solution is slowly added into the cyclodextrin Tween 80 aqueous solution, per minute to add 1 liter or so, total 20 minutes time of addition.Add
Mixing is finished, then keeping temperature continues to stir 60 minutes.Stirring finishes 60 DEG C of vacuum distillations under 0.1 atmospheric pressure vacuum and reclaimed
Ethanol, recovery is finished, and is spray-dried with 120 DEG C of hot blast temperature, is obtained leaf of bamboo antioxidant cyclodextrin inclusion compound 7708g.
Using the method for embodiment 1, after testing, general flavone inclusion rate is up to 88%, through adding in 60 DEG C of insulating boxs for gained inclusion compound
Fast oxidation test, the 15th day leaf of bamboo antioxidant inclusion compound removes free radical rate and retains 94%, and raw material is removed free radical rate and retained
79%, the 20th day leaf of bamboo antioxidant inclusion compound removes free radical rate and retains 86%, and raw material removes free radical rate reservation 61%, the
30 days leaf of bamboo antioxidant inclusion compounds retain 67%, and raw material removes free radical rate and retains 31%.
Leaf of bamboo antioxidant cyclodextrin inclusion compound 1.0g is weighed, 10ml deionized waters is added, is stirred at room temperature, can be complete
It is dissolved as clear solution.Sample solution is compared, no leaf of bamboo taste through tasting with 40% ethanol solution of leaf of bamboo antioxidant.
Embodiment 4：
Weighing 1000 grams of leaf of bamboo antioxidant, (its general flavone content of spectrophotometry is 30%, purchased from Shaanxi Kang Yue
Bio tech ltd), it is dissolved in 30 liters of ethanol waters of volumetric concentration 50%, stirring makes it fully dissolve, and bamboo is made
Leaf aqueous antioxidant solution.Weigh 5000 grams of food-grade cyclodextrin (being purchased from Wuxi City Jian Xing starch-based products Co., Ltd), dissolving
In 160 liters of deionized waters, then 2.0 grams of food grade emulsifier tweens 80 are weighed, be dissolved in cyclodextrin aqueous solution, in enamel still
Stir, form the cyclodextrin Tween 80 aqueous solution, and be heated to 50 DEG C, by leaf of bamboo antioxygen in being stirred continuously under constant temperature
Agent solution is slowly added into the cyclodextrin Tween 80 aqueous solution, per minute to add 1 liter or so, total 20 minutes time of addition.Plus
Enter mixing to finish, then keeping temperature continues to stir 40 minutes.Stirring finishes under 0.1 atmospheric pressure vacuum 60 DEG C and is evaporated in vacuo back
Ethanol is received, recovery is finished, be spray-dried with 130 DEG C of hot blast temperature, obtain leaf of bamboo antioxidant cyclodextrin inclusion compound 5705g.
Using the method for embodiment 1, after testing, general flavone inclusion rate is up to 87%, through adding in 60 DEG C of insulating boxs for gained inclusion compound
Fast oxidation test, the 15th day leaf of bamboo antioxidant inclusion compound removes free radical rate and retains 93%, and raw material is removed free radical rate and retained
79%, the 20th day leaf of bamboo antioxidant inclusion compound removes free radical rate and retains 85%, and raw material removes free radical rate reservation 60%, the
30 days leaf of bamboo antioxidant inclusion compounds retain 65%, and raw material removes free radical rate and retains 30%.
Leaf of bamboo antioxidant cyclodextrin inclusion compound 1.0g is weighed, 10ml deionized waters is added, is stirred at room temperature, can be complete
It is dissolved as clear solution.Sample solution is compared, no leaf of bamboo taste through tasting with 40% ethanol solution of leaf of bamboo antioxidant.
Claims (7)
1. a kind of method for improving leaf of bamboo antioxidant stability, it is characterised in that methods described is：Leaf of bamboo antioxidant is molten
Leaf of bamboo antioxidant solution is made in volumetric concentration 30-50% ethanol waters；Again by after cyclodextrin deionized water dissolving
Emulsifying agent is added, mixes, cyclodextrin solution is made；Cyclodextrin solution is heated to 30-60 DEG C, leaf of bamboo antioxidant is slowly added to
Stirring reaction 30-60min after solution, completion of dropping, reaction solution vacuum distillation removes ethanol, dries, and obtains leaf of bamboo antioxidant
Cyclodextrin inclusion compound, realizes the raising of leaf of bamboo antioxidant stability；The emulsifying agent is Tween 80 or sorbester p17；The leaf of bamboo
Antioxidant is 1 with cyclodextrin, emulsifying agent mass ratio:1-10：0.001-0.1；The ethanol water volumetric usage is with the leaf of bamboo
Antioxidant quality is calculated as 20-40L/kg, and the deionized water volumetric usage is calculated as 20-50L/Kg with cyclodextrin quality.
2. the method for leaf of bamboo antioxidant stability is improved as claimed in claim 1, it is characterised in that the leaf of bamboo antioxidant
Middle flavones mass content is 25-40%.
3. the method for leaf of bamboo antioxidant stability is improved as claimed in claim 1, it is characterised in that the ethanol water body
Product consumption is calculated as 20L/Kg with leaf of bamboo antioxidant quality.
4. the method for leaf of bamboo antioxidant stability is improved as claimed in claim 1, it is characterised in that the deionized water volume
Consumption is calculated as 25L/Kg with cyclodextrin quality.
5. the method for leaf of bamboo antioxidant stability is improved as claimed in claim 1, it is characterised in that the leaf of bamboo antioxidant
Solution rate of addition is 1L/min.
6. the method for leaf of bamboo antioxidant stability is improved as claimed in claim 1, it is characterised in that the reaction solution exists
0.1Pa, at 60 DEG C vacuum distillation remove ethanol, then be spray-dried at 120-150 DEG C.
7. the method for leaf of bamboo antioxidant stability is improved as claimed in claim 1, it is characterised in that the leaf of bamboo antioxidant
It is 1 with cyclodextrin, emulsifying agent mass ratio:4-7：0.002-0.005.
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