CN105361182A - Composite stabilizer formulation containing suaeda salsa anthocyanin and application of composite stabilizer formulation - Google Patents
Composite stabilizer formulation containing suaeda salsa anthocyanin and application of composite stabilizer formulation Download PDFInfo
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- CN105361182A CN105361182A CN201510660910.7A CN201510660910A CN105361182A CN 105361182 A CN105361182 A CN 105361182A CN 201510660910 A CN201510660910 A CN 201510660910A CN 105361182 A CN105361182 A CN 105361182A
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- 241000586290 Suaeda salsa Species 0.000 title claims abstract description 31
- 239000000203 mixture Substances 0.000 title abstract description 9
- 235000010208 anthocyanin Nutrition 0.000 title abstract 7
- 229930002877 anthocyanin Natural products 0.000 title abstract 7
- 239000004410 anthocyanin Substances 0.000 title abstract 7
- 150000004636 anthocyanins Chemical class 0.000 title abstract 7
- 238000009472 formulation Methods 0.000 title abstract 5
- 239000006084 composite stabilizer Substances 0.000 title abstract 3
- 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 32
- 238000000034 method Methods 0.000 claims abstract description 21
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 16
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 16
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 16
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 16
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims abstract description 16
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 16
- 239000011718 vitamin C Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229930014669 anthocyanidin Natural products 0.000 claims description 65
- 150000001452 anthocyanidin derivatives Chemical class 0.000 claims description 65
- 235000008758 anthocyanidins Nutrition 0.000 claims description 65
- 238000000605 extraction Methods 0.000 claims description 52
- 239000000284 extract Substances 0.000 claims description 19
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 15
- 229960005055 sodium ascorbate Drugs 0.000 claims description 15
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000002250 absorbent Substances 0.000 claims description 10
- 230000002745 absorbent Effects 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 8
- 208000003556 Dry Eye Syndromes Diseases 0.000 claims description 7
- 230000006641 stabilisation Effects 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 5
- 239000000287 crude extract Substances 0.000 claims description 4
- 238000011105 stabilization Methods 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 238000003306 harvesting Methods 0.000 claims description 3
- 239000000049 pigment Substances 0.000 abstract description 39
- 239000003381 stabilizer Substances 0.000 abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 238000005286 illumination Methods 0.000 abstract description 5
- 230000003111 delayed effect Effects 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 241000196324 Embryophyta Species 0.000 abstract description 3
- 235000000346 sugar Nutrition 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 1
- 241000201912 Suaeda Species 0.000 abstract 1
- 235000021310 complex sugar Nutrition 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 230000000694 effects Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- 239000003513 alkali Substances 0.000 description 13
- 238000004040 coloring Methods 0.000 description 13
- 238000002835 absorbance Methods 0.000 description 11
- 230000036541 health Effects 0.000 description 9
- 238000011160 research Methods 0.000 description 7
- 235000013305 food Nutrition 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- VEVZSMAEJFVWIL-UHFFFAOYSA-O cyanidin cation Chemical compound [O+]=1C2=CC(O)=CC(O)=C2C=C(O)C=1C1=CC=C(O)C(O)=C1 VEVZSMAEJFVWIL-UHFFFAOYSA-O 0.000 description 2
- -1 cyanine glycoside Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 235000002864 food coloring agent Nutrition 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000004089 microcirculation Effects 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229940123457 Free radical scavenger Drugs 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000017442 Retinal disease Diseases 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000002490 cerebral effect Effects 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 235000007336 cyanidin Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 208000001491 myopia Diseases 0.000 description 1
- 230000004379 myopia Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- ANRHNWWPFJCPAZ-UHFFFAOYSA-M thionine Chemical compound [Cl-].C1=CC(N)=CC2=[S+]C3=CC(N)=CC=C3N=C21 ANRHNWWPFJCPAZ-UHFFFAOYSA-M 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- 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)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a stabilizer formulation containing suaeda salsa anthocyanin. The stabilizer formulation is prepared from, by mass, 0.05% to 0.075% of vitamin C, 0.015% to 0.03% of vitamin C sodium, 0.04% to 0.06% of sodium benzoate and the balance suaeda salsa anthocyanin extracting solution. The invention further discloses an application of the formulation. According to composite stabilizer containing anthocyanin, it is proved through experiments that after the stabilizer is added, the degradation function of temperature, illumination, the power of hydrogen, a reducing agent and the like on pigments is effectively delayed. The invention further provides a method for extracting natural pigment anthocyanin with a biological healthcare function from halophyte suaeda salsa which is widely distributed on coastal mud flat salinate fields and stabilizing the natural pigment anthocyanin. The defects that an existing anthocyanin extracting raw material source is limited, an extracting process is complex, and energy consumption is high are overcome, the sugar content of saline land common seepweed herb plants is low, no complex sugar removing process treatment is needed, and the technological process is simplified.
Description
Technical field
The present invention relates to technical field of health care food, be specifically related to a kind of combinative stability agent prescription containing Suaeda salsa anthocyanidin and application thereof.
Background technology
Suaeda salsa is a kind of typical euhalophyte, the salt licks such as Coastal beach extensively distributes, is a kind of natural resources having very much development potentiality, has very large economic benefit, ecological benefits and social benefit.Research confirms that abundant haematochrome contained in Suaeda salsa is cyanine glycoside pigment.
Along with socioeconomic development, current people are to the pay attention to day by day of health, and natural colouring matter replaces synthetic dyestuff to become trend of the times.Anthocyanidin is among the people as a kind of natural food colour Long-Time Service in China.Research also confirms, anthocyanidin also has the regeneration of promotion erythropsin, improve microcirculation, thus in treatment myopia and retinal disease, achieve good efficacy, while anthocyanidin pair and the curative effect of microcirculation disorder diseases related as diseases such as diabetes, hypertension, artery sclerosis and cerebral circulatory disorders also comparatively remarkable.Italy and Germany have carried out the research of extraction cyanidin extract in medicine.In addition, have research data to show, anthocyanidin is a kind of free radical scavenger, can significantly improve body anti-oxidation function.In addition, anthocyanidin can keep and increase the activity of vitamin in human body, is a kind of vitamin synergist.
From the viewpoint of to health and security, use the natural colouring matter anthocyanidin with health care to be ideal, but also there is the restriction of some factors at present: 1) extract natural colouring matter anthocyanidin raw material sources limited.2) due in plant often containing a large amount of carbohydrate, extraction process is more loaded down with trivial details and consume energy more.3) natural colouring matter extracts from natural plants, and due to complicated component, what have is also together with each other, therefore often have other compositions in extraction pigment, so use amount is more relative to synthetic dyestuff, owing to there being the impact of the composition that coexists, sometimes there is peculiar smell.4) the natural colouring matter color range extracted does not reach application requirement in the food industry.5) pigment had is different with pH value, and stability is also different, sometimes has the change of tone, in processing and the process of circulation, because the impact of extraneous factor is easily deteriorated.
Summary of the invention
Goal of the invention: for the limitation and the deficiencies in the prior art that use natural colouring matter at present, the invention provides that a kind of wide material sources, biomass are large, the simple pigment of economy, natural goods composition extracts raw material, extraction step is simple, consume energy few extracting method, and through separation purifying technique, solve the bottleneck problem using natural colouring matter, for the resources development and utilization promoting the use of natural food colour and halophytes Suaeda salsa provides the approach had a extensive future.Trial production has gone out the agent of a kind of anthocyanidin combinative stability simultaneously, and test proves, has effectively delayed the degradation to pigment such as temperature, illumination, acid-base value, reducing agent after adding stabilizing agent.
Technical scheme: in order to solve the problems of the technologies described above, the invention provides a kind of combinative stability agent prescription containing Suaeda salsa anthocyanidin, comprise following component according to mass percent: vitamin C 0.05 ~ 0.075%, sodium ascorbate 0.015 ~ 0.03%, Sodium Benzoate 0.04 ~ 0.06%, surplus is Suaeda salsa anthocyanidin extract.
Preferably, comprise following component according to mass percent: vitamin C 0.05%, sodium ascorbate 0.015%, Sodium Benzoate 0.04%, surplus is Suaeda salsa anthocyanidin extract.
Preferably, comprise following component according to mass percent: vitamin C 0.075%, sodium ascorbate 0.03%, Sodium Benzoate 0.06%, surplus is Suaeda salsa anthocyanidin extract.
A kind of Suaeda salsa anthocyanidin stabilization process, comprises the following steps:
1) pretreatment of raw material: the fresh soda of harvesting is fluffy removes root, cleans, dries, shred, and crosses 40 mesh sieves, and obtaining dry-eye disease, to be stored in dry lucifuge place for subsequent use;
2) lixiviate: get the above-mentioned pretreated dry-eye disease of 1g, add 40 ~ 50mL deionized water or organic solvent, controlling extraction temperature is 40 ~ 50 DEG C, extraction time controls at 30 ~ 50min, centrifugal 10min, after getting its supernatant by above step again lixiviate once, merge twice lixiviate supernatant;
3) purifying: the supernatant extracted through above-mentioned technique is carried out sorption and desorption through macroporous absorbent resin, with crude extract stoste loading, adsorption time 1.5 ~ 2h take volume fraction as the ethanolic solution desorb of 50%, time 1 ~ 1.5h, obtains the anthocyanidin extract after purifying;
4) stabilisation: add vitamin C 0.05 ~ 0.075% according to formula according to claim 1 in anthocyanidin extract, sodium ascorbate 0.015 ~ 0.03%, Sodium Benzoate 0.04 ~ 0.06% obtain the Suaeda salsa anthocyanidin after stable.
Further, above-mentioned steps 2) in organic solvent be one in ethanolic solution, absolute ethyl alcohol, ether, chloroform, acetone, glacial acetic acid.
Further, above-mentioned steps 4) in temperature be 35 ~ 55 DEG C.
Further, above-mentioned ethanolic solution mass percent concentration is 5% ~ 20%.
Further, above-mentioned steps 2) in liquid-solid ratio be 40 ~ 50:1 (mL/g).
Further, above-mentioned steps 2) liquid-solid ratio is 40mL/g, extraction temperature 40 DEG C, extraction time 50 minutes.
Further, above-mentioned steps 3) in macroporous absorbent resin be AB-8 type macroporous absorbent resin.
Further, above-mentioned steps 3) adsorption flow rate is 1mL/min, loading volume 60mL, elution speed 2.5mL/min.
Beneficial effect: the invention provides a kind of method extracting the natural colouring matter anthocyanidin with biological health function in halophytes Suaeda salsa of extensively distribution from Coastal beach salt lick, solve current anthocyanidin extract raw material sources limited, extraction process is loaded down with trivial details and the shortcoming of big energy-consuming, and Suaeda salsa plant sugar content is low, can not carry out loaded down with trivial details except sugared PROCESS FOR TREATMENT, simplify technological process.Simultaneously this technique determines by test the optimum resin that AB-8 type macroporous absorbent resin is purifying pigment, and through purification process, cyanine plain color valency increases to 5.6, substantially exceed country about natural colouring matter in food additives 3.0 standard-required.Trial production has gone out the agent of a kind of anthocyanidin combinative stability simultaneously, and test proves, has effectively delayed the degradation to pigment such as temperature, illumination, acid-base value, reducing agent after adding stabilizing agent.
Accompanying drawing explanation
Fig. 1 Suaeda salsa anthocyanidin UV-vis absorption spectrum;
Fig. 2 liquid-solid ratio is on the impact of the fluffy anthocyanidin extraction effect of alkali;
Fig. 3 temperature is on the impact of the fluffy anthocyanidin extraction effect of alkali;
Fig. 4 extraction time is on the impact of the fluffy anthocyanidin extraction effect of alkali;
Fig. 5 extraction time is on the impact of the fluffy anthocyanidin extraction effect of alkali.
Detailed description of the invention
Below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1
Add in food the fluffy middle extraction of alkali there is the natural colouring matter anthocyanidin of biological health function time add the colorant stabilizer of following component: the Sodium Benzoate of the sodium ascorbate+0.04% of 0.05% vitamin C+0.03%, increases pigment stability.
Embodiment 2
Add in food the fluffy middle extraction of alkali there is the natural colouring matter anthocyanidin of biological health function time add the colorant stabilizer of following component: the Sodium Benzoate of the sodium ascorbate+0.06% of 0.05% vitamin C+0.015%, increases pigment stability.
Embodiment 3
Add in food the fluffy middle extraction of alkali there is the natural colouring matter anthocyanidin of biological health function time add the colorant stabilizer of following component: the Sodium Benzoate of the sodium ascorbate+0.04% of 0.075% vitamin C+0.03%, increases pigment stability.
Embodiment 4
Add in food the fluffy middle extraction of alkali there is the natural colouring matter anthocyanidin of biological health function time add the colorant stabilizer of following component: the Sodium Benzoate of the sodium ascorbate+0.06% of 0.075% vitamin C+0.015%, increases pigment stability.
Experimental example 1:
A kind of Suaeda salsa anthocyanidin stabilization process, comprises the following steps:
1) pretreatment of raw material: the fresh soda of harvesting is fluffy removes root, cleans, dries, shred, and crosses 40 mesh sieves, and obtaining dry-eye disease, to be stored in dry lucifuge place for subsequent use;
2) lixiviate: get the above-mentioned pretreated dry-eye disease of 1g, add 40mL deionized water or organic solvent, controlling extraction temperature is 40 DEG C, extraction time controls at 30min, centrifugal 10min, after getting its supernatant by above step again lixiviate once, merge twice lixiviate supernatant;
3) purifying: the supernatant extracted through above-mentioned technique is carried out sorption and desorption through macroporous absorbent resin, with crude extract stoste loading, adsorption time 1.5 ~ 2h take volume fraction as the ethanolic solution desorb of 50%, time 1 ~ 1.5h, obtains the anthocyanidin extract after purifying;
4) stabilisation: add vitamin C according to the formula described in embodiment 1 ~ 4 in anthocyanidin extract, sodium ascorbate, Sodium Benzoate obtain the Suaeda salsa anthocyanidin after stable.
Experimental example 2: the determination of extractant
Getting 10 parts of above-mentioned dry-eye disease of 0.1g adds in 20mL deionized water, 5% ethanol, 10% ethanol, 20% ethanol, 50% ethanol, absolute ethyl alcohol, ether, chloroform, acetone, glacial acetic acid respectively, under room temperature, dark place lixiviate 30min, suction filtration obtains filtrate, proceed in colorimetric cylinder, observe liquid color.Color is darker, and extraction efficiency is larger.Get 10mL with the darkest person of color and be diluted to suitable multiple, measure ultraviolet-visible absorption spectroscopy, determine the maximum absorption wavelength of its pigment.
Research shows, Suaeda salsa anthocyanidin is insoluble in organic solvent, the organic solvent that soluble in water and water content is high, the extractability of 5% ethanolic solution, 10% ethanolic solution, 20% ethanolic solution, deionized water is stronger, but consider the needs (namely should simplify step as far as possible, reduce costs while guarantee extraction efficiency) of actual production, deionized water or 5% ethanolic solution should be chosen as digestion agent.Through spectrophotometer scanning after extract suitably dilutes, determine that the maximum absorption wavelength of anthocyanidin solution is 540nm.
The dissolving situation of the fluffy anthocyanidin of table 4 alkali in different extractant
Upper table data show, Suaeda salsa anthocyanidin is insoluble in organic solvent, the organic solvent that soluble in water and water content is high, and the extractability of 5% ethanolic solution, 10% ethanolic solution, 20% ethanolic solution, deionized water is stronger.
Fig. 1 shows, deionized water and 50% ethanol extract have one to absorb peak at 540nm place, therefore the absorption spectrum of the fluffy anthocyanidin of alkali is 540nm, meets the spectral region of cyanine glycoside pigment.
Experimental example 3 lixiviate parameter single factor experiment
Liquid-solid ratio: test shows, along with the increase of extract and dry powder sample liquid-solid ratio, the absorbance of pigment solution raises gradually, and when liquid-solid ratio is greater than 40 ~ 50:1, curve tends towards stability, and absorbance changes little.Consider the burden when increase of digestion agent consumption can increase cost and later stage concentrate drying, therefore liquid-solid ratio is chosen as 40 ~ 50:1 (mL/g) left and right.
Fig. 2 shows, when liquid-solid ratio is greater than 50:1, curve tends towards stability, and absorbance changes little.Consider the burden when increase of digestion agent consumption can increase cost and later stage concentrate drying, therefore liquid-solid ratio is chosen as 40 ~ 50:1 (mL/g) left and right and is advisable.
Extraction temperature: test shows, along with the rising of temperature, pigment solution absorbance has a process obviously risen, and pigment recovery rate increases.And after 50 DEG C, curve is tending towards declining on the contrary, this heat resistance due to pigment is bad, and the high temperature structure of pigment, affects the stability of pigment.Therefore, the Extracting temperature of lixiviate is unsuitable too high, more suitable with 40 ~ 50 DEG C.
Fig. 3 shows, along with the rising of temperature, pigment solution absorbance first rises, and after 50 DEG C, curve is tending towards declining on the contrary.Therefore, the Extracting temperature of lixiviate is unsuitable too high, more suitable with 40 ~ 50 DEG C.
Extraction time: test shows, with the change of extraction time, solution absorbance is slow ascendant trend, and after 120min, curve tends towards stability, and absorbance no longer raises.This test raw material degree of grinding is comparatively thin, is conducive to the stripping of pigment, and extraction time is not so good as liquid-solid ratio to the impact of extraction effect and extraction temperature impact is remarkable.
Fig. 4 shows, with the change of extraction time, solution absorbance is slow ascendant trend, and this test raw material degree of grinding is comparatively thin, is conducive to the stripping of pigment, and extraction time is not so good as liquid-solid ratio to the impact of extraction effect and extraction temperature impact is remarkable.
Extracting times: compare absorbance change after the filtrate of compare lixiviate 1 time, 2 times and 3 times adjusts to same volume, along with increasing of extracting times, the absorbance of leaching liquor increases gradually, but amplitude of variation slows down.After lixiviate twice, recovery rate amplification is less, and the concentrated and actual production time consideration from the later stage, lixiviate is advisable for twice.
After Fig. 5 shows lixiviate twice, recovery rate amplification is less, and from the later stage, concentrated and actual production time is considered, lixiviate is advisable for twice.
The optimization of experimental example 4 extracting technology
According to single factor experiment, select liquid-solid ratio, extraction temperature and extraction time to be principal element, adopt the optimization of orthogonal test research extraction process.Result of the test shows that on the impact order of the fluffy anthocyanidin extraction effect of alkali be liquid-solid ratio > extraction temperature > extraction time, and optimum extraction process is liquid-solid ratio 40mL/g, extraction temperature 40 DEG C, extraction time 50 minutes.
Table 5 alkali fluffy anthocyanidin optimal extraction technology orthogonal test factor level
Adopt the optimization of orthogonal test research extraction process.Result shows that on the impact order of the fluffy anthocyanidin extraction effect of alkali be liquid-solid ratio > extraction temperature > extraction time, and optimum extraction process is liquid-solid ratio 40mL/g, extraction temperature 40 DEG C, extraction time 50 minutes.
Experimental example 5 anthocyanidin purifying
Macroporous absorbent resin is a kind of high molecular polymer, has macroreticular structure and larger specific area, can from solution selectable adsorbed target composition, thus reach the effect of separation and purification.Be characterized in that physicochemical properties are stablized, selective adsorption capacity is strong, and adsorption rate is fast, and the simple cost of technique is low, renewable use etc.
The macroporous absorbent resin of different model, opposed polarity is chosen in test, after the alcohol immersion of 95%, cleans with distilled water.According to each resin, the adsorption rate of anthocyanidin extracted, desorption efficiency are determined to the resin model of applicable purifying.By purifying process that is static, dynamic experiment determination pigment.Calculate yield and look valency.More dissimilar macroporous absorbent resin, to Static Adsorption, the desorption ability of pigment, determines that AB-8 type macroporous absorbent resin is the optimum resin of purifying pigment.Static test result shows: under room temperature, and with crude extract stoste loading, adsorption time 1.5 ~ 2h take volume fraction as the ethanolic solution desorb of 50%, time 1 ~ 1.5h.Dynamic test shows: optimal adsorption flow velocity is 1mL/min, loading volume 60mL, elution speed 2.5mL/min.Pigment yield 2.2%, after purifying, pigment powder is kermesinus, and look valency 1.3 increases to 5.6 before purifying.
Experimental example 7
After adding stabilizing agent, following form is shown in the impact of anthocyanidin solution on temperature, illumination, pH value, reducing agent etc.:
Table 6 temperature is on the impact of pigment stability
Upper table data show, the heat resistance of anthocyanidin is poor, can accelerate along with the rising Pigment degradation speed of temperature.Stabilizing agent is added to delaying Pigment degradation DeGrain when low temperature and high temperature.But when 35-55 DEG C, add the stablizing effect of stabilizing agent to anthocyanidin obvious.
Table 7 illumination is on the impact of pigment stability
Upper table data show, after adding stabilizing agent, have effectively delayed anthocyanidin degraded, improve the stability of anthocyanidin to light.
The impact of table 8 reducing agent on pigment stability (adds variable concentrations Na
2sO
3)
Upper table data show, the stability influence of reducing agent to anthocyanidin is larger.Along with reductant concentration increase and the prolongation of action time, absorbance declines also faster.After adding stabilizing agent, anthocyanidin solution can improve the tolerance of pigment to the reducing agent of low concentration effectively.
Table 9 vitamin C consumption is on the impact of anthocyanidin stability
Upper table data show that the vitamin C stablizing effect of interpolation 0.05% ~ 0.075% is best, can delay the oxidation of pigment preferably.
Table 10 sodium ascorbate consumption is on the impact of anthocyanidin stability
Upper table data show that the sodium ascorbate stablizing effect of interpolation 0.015% ~ 0.03% is best, can delay the oxidation of pigment preferably.
Table 11 Sodium Benzoate consumption is on the impact of anthocyanidin stability
Upper table data show that the Sodium Benzoate stablizing effect of interpolation 0.04% ~ 0.06% is best, can delay the oxidation of pigment preferably.
Claims (5)
1. the combinative stability agent prescription containing Suaeda salsa anthocyanidin, it is characterized in that, comprise following component according to mass percent: vitamin C 0.05 ~ 0.075%, sodium ascorbate 0.015 ~ 0.03%, Sodium Benzoate 0.04 ~ 0.06%, surplus is Suaeda salsa anthocyanidin extract.
2. a kind of combinative stability agent prescription containing Suaeda salsa anthocyanidin according to claim 1, it is characterized in that, comprise following component according to mass percent: vitamin C 0.05%, sodium ascorbate 0.015%, Sodium Benzoate 0.04%, surplus is Suaeda salsa anthocyanidin extract.
3. a kind of combinative stability agent prescription containing Suaeda salsa anthocyanidin according to claim 1, it is characterized in that, comprise following component according to mass percent: vitamin C 0.075%, sodium ascorbate 0.03%, Sodium Benzoate 0.06%, surplus is Suaeda salsa anthocyanidin extract.
4. a Suaeda salsa anthocyanidin stabilization process, is characterized in that, comprises the following steps:
1) pretreatment of raw material: the fresh soda of harvesting is fluffy removes root, cleans, dries, shred, and crosses 40 mesh sieves, and obtaining dry-eye disease, to be stored in dry lucifuge place for subsequent use;
2) lixiviate: get the above-mentioned pretreated dry-eye disease of 1g, add 40 ~ 50mL deionized water or organic solvent, controlling extraction temperature is 40 ~ 50 DEG C, extraction time controls at 30 ~ 50min, centrifugal 10min, after getting its supernatant by above step again lixiviate once, merge twice lixiviate supernatant;
3) purifying: the supernatant extracted through above-mentioned technique is carried out sorption and desorption through macroporous absorbent resin, with crude extract stoste loading, adsorption time 1.5 ~ 2h take volume fraction as the ethanolic solution desorb of 50%, time 1 ~ 1.5h, obtains the anthocyanidin extract after purifying;
4) stabilisation: add vitamin C 0.05 ~ 0.075% according to formula according to claim 1 in anthocyanidin extract, sodium ascorbate 0.015 ~ 0.03%, Sodium Benzoate 0.04 ~ 0.06% obtain the Suaeda salsa anthocyanidin after stable.
5. a kind of Suaeda salsa anthocyanidin stabilization process according to claim 4, it is characterized in that, the temperature in step 4) is 35 ~ 55 DEG C.
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