CN105707881A - Coenzyme Q10 aqueous dispersion and preparing method thereof - Google Patents
Coenzyme Q10 aqueous dispersion and preparing method thereof Download PDFInfo
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- CN105707881A CN105707881A CN201610107113.0A CN201610107113A CN105707881A CN 105707881 A CN105707881 A CN 105707881A CN 201610107113 A CN201610107113 A CN 201610107113A CN 105707881 A CN105707881 A CN 105707881A
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- Prior art keywords
- coenzyme
- salanesol
- aqueous dispersion
- obtains
- preparation
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- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 title claims abstract description 77
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 235000017471 coenzyme Q10 Nutrition 0.000 title claims abstract description 74
- 229940110767 coenzyme Q10 Drugs 0.000 title claims abstract description 73
- 239000006185 dispersion Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229920002472 Starch Polymers 0.000 claims abstract description 14
- 239000006184 cosolvent Substances 0.000 claims abstract description 14
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 14
- 235000019698 starch Nutrition 0.000 claims abstract description 14
- 239000008107 starch Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000000199 molecular distillation Methods 0.000 claims description 28
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 125000001891 dimethoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 21
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 21
- 150000002924 oxiranes Chemical class 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 14
- 108010010803 Gelatin Proteins 0.000 claims description 13
- 229920000159 gelatin Polymers 0.000 claims description 13
- 239000008273 gelatin Substances 0.000 claims description 13
- 235000019322 gelatine Nutrition 0.000 claims description 13
- 235000011852 gelatine desserts Nutrition 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 244000061458 Solanum melongena Species 0.000 claims description 10
- 235000002597 Solanum melongena Nutrition 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- WQZGKKKJIJFFOK-SVZMEOIVSA-N (+)-Galactose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-SVZMEOIVSA-N 0.000 claims description 8
- 238000011282 treatment Methods 0.000 claims description 8
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims description 7
- 239000003463 adsorbent Substances 0.000 claims description 7
- 125000001246 bromo group Chemical group Br* 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 7
- 239000003480 eluent Substances 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 7
- 238000006266 etherification reaction Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000003208 petroleum Substances 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 238000007127 saponification reaction Methods 0.000 claims description 7
- 229940055329 tobacco leaf extract Drugs 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 7
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 6
- 235000010489 acacia gum Nutrition 0.000 claims description 6
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 239000008101 lactose Substances 0.000 claims description 6
- 238000002242 deionisation method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- 150000001720 carbohydrates Chemical class 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920000136 polysorbate Polymers 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- -1 sucrose ester Chemical class 0.000 claims description 4
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 3
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 3
- 229960000502 poloxamer Drugs 0.000 claims description 3
- 229920001983 poloxamer Polymers 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 25
- 239000000243 solution Substances 0.000 description 13
- 235000013305 food Nutrition 0.000 description 11
- 239000000047 product Substances 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 235000013402 health food Nutrition 0.000 description 3
- 230000036039 immunity Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 102000005606 Activins Human genes 0.000 description 1
- 108010059616 Activins Proteins 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 208000033042 Somatoform disorder cardiovascular Diseases 0.000 description 1
- 229930003448 Vitamin K Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000488 activin Substances 0.000 description 1
- 238000009098 adjuvant therapy Methods 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 208000015606 cardiovascular system disease Diseases 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 210000003470 mitochondria Anatomy 0.000 description 1
- 230000003387 muscular Effects 0.000 description 1
- 208000009157 neurocirculatory asthenia Diseases 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- SHUZOJHMOBOZST-UHFFFAOYSA-N phylloquinone Natural products CC(C)CCCCC(C)CCC(C)CCCC(=CCC1=C(C)C(=O)c2ccccc2C1=O)C SHUZOJHMOBOZST-UHFFFAOYSA-N 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 229960004747 ubidecarenone Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 235000019168 vitamin K Nutrition 0.000 description 1
- 239000011712 vitamin K Substances 0.000 description 1
- 150000003721 vitamin K derivatives Chemical class 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 229940046010 vitamin k Drugs 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/35—Ketones, e.g. benzophenone
- A61K8/355—Quinones
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- 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
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Dermatology (AREA)
- Emergency Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Medicinal Preparation (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a coenzyme Q10 aqueous dispersion and a preparing method thereof. The preparing method comprises the following steps that 1, raw materials are prepared, wherein coenzyme Q10, gum substance, sugar, an emulsifying agent, soluble starch, cosolvent and water are prepared; 2, water is added into the gum substance to dissolve the gum substance, the soluble starch, the sugar and the emulsifying agent are added, and the mixture is heated, dissolved and stirred uniformly for use; 3, the cosolvent is heated and dissolved, and then coenzyme Q10 is added, heated and dissolved for use; 4, pressurizing is carried out, materials treated in the step two and the step three are placed into a high-pressure tank and pressurized to 4 kg/cm<2> to enable pressure to be uniform, the pressure is kept for 5-10 min, and then normal pressure is restored within 1-3 seconds, so that mixed liquor is obtained; 5, the mixed liquor obtained in the step four is dried in a spraying mode, so that coenzyme Q10 aqueous dispersion powder is obtained.
Description
Technical field
The present invention relates to biological technical field, a kind of coenzyme Q10 aqueous dispersion and preparation thereof
Method.
Background technology
Coenzyme Q10, English name: COENZYME Q10, CAS No.303-98-0, molecular formula C59H90O4,
Molecular weight 863.36, for yellow to orange-yellow crystalline powder, odorless, tasteless, is shown in that light easily decomposes,
In ethanol and micro dissolution, insoluble in water.It has another name called Ubidecarenone, is a kind of fat-soluble quinone, its knot
Structure is similar to vitamin K, because the degree of polymerization of the side chain polyisoamylene base on its parent nucleus six is 10
And gain the name, it is a kind of quinone cyclics.Coenzyme Q10 is the indispensable important element of human life
One of, can human activin cell and the nutrition of cellular energy, have raising body immunity, strengthen anti-
The functions such as oxidation, slow down aging and enhancing human activity, are medically widely used in cardiovascular system diseases,
Extensively use it for nutrient and healthcare products and food additive both at home and abroad.
Modern pharmacological research shows, coenzyme Q10 mainly has two effects: one is at nutrient
Matter plays an important role during being converted into energy in mitochondrion；Two is to have obvious lipotropism matter mistake
Oxidation.Coenzyme Q10 application clinically mainly has: defying age, protection skin, the protection heart
Dirty, resisting fatigue, enhancing muscular energy, resisting hypertension, treating chronic effort syndrome.
The research application of state's coenzyme Q 10 is main at two aspects at present: one is for cosmetics, auxiliary
Enzyme Q10 can remove human free radical because reaching the beautification function of defying age；Two is for pharmaceuticals industry,
Coenzyme Q10 can the disease such as adjuvant therapy of cardiovascular.Coenzyme Q10 is widely used in Japan: day calendar year 2001
Coenzyme Q10 is approved as " health food " for beauty food, resisting fatigue food by this Health and human services department bureau of drug
In the food such as product and beverage.Japanese health ministry medicine office also announced in 2005, and coenzyme Q10 has
Well health care, and confirmed with application by years of researches.At present, Japanese every day is about
12000000 people's long-term takings contain preparation and the health product of coenzyme Q10.Chinese food pharmaceuticals administration
Office is also used for health food in approval coenzyme Q10 in 2006, is mainly used in enhancing immunity, antioxygen
Change, auxiliary adjustment of blood fat and alleviating physical fatigue.
Human body can be by absorbing and these two approach of internal manufacture obtain coenzyme Q10 from food, but carefully
The coenzyme Q10 that born of the same parents are obtained by food.Content cannot meet far away the needs of human normal physiological function,
Therefore, either healthy population or Disease, it is required for supplementing coenzyme Q10.But due to coenzyme
Q10 molecular weight is big, water solublity is excessively poor, therefore together should eat, so with the meals containing fat
Its absorption can be increased.But, wherein the absorption in intestinal is the slowest, oral coenzyme Q10.Biological
Availability is the most relatively low.The safest raising coenzyme Q10.Bioavailability becomes in vivo
Focus for external Recent study.It is the biological profit of a kind of raising that coenzyme Q10 is prepared as aqueous dispersion
The method of expenditure, domestic patent employs the antioxidant protection coenzyme Q10 of physiologically active, has one
Fixed potential safety hazard.Foreign patent is mainly Japan Patent, the substantial amounts of Sucrose Fatty Acid Ester of W02006134970
Fat acid esters makees emulsifying agent, and cost is high, and consumption is excessive, has potential, unknown unsafe factor.
Summary of the invention
It is an object of the invention to provide a kind of coenzyme Q10 aqueous dispersion and preparation method thereof, with useless cigarette
Leaf be raw material extract synthesis coenzyme Q10 be raw material, be aided with whole edible gelatin substance, emulsifying
The material such as agent, cosolvent, a kind of biological utilisation degree of synthesis is high, the coenzyme Q10 that compliance is good
Aqueous dispersion.
The present invention is achieved through the following technical solutions, and specifically includes following steps:
1) raw material prepares: get out coenzyme Q10, gelatin substance, sugar, emulsifying agent, solubility shallow lake
Powder, cosolvent, water；
2) gelatin substance is dissolved in water, adds soluble starch, saccharide, emulsifying agent, heating
Dissolve, stir, standby；
3) by cosolvent heating for dissolving, coenzyme Q10 is added, heating for dissolving, standby；
4) pressurized treatments: by step 2) and step 3) process after material, put in pressure pan,
It is forced into 4kg/cm2So that it is pressure is uniform, and keeps 5-10min, then often recovers in 1-3s
Pressure, obtains mixed liquor；
5) by step 4) mixed liquor that obtains is spray-dried, and obtains coenzyme Q10 aqueous dispersion powder；
Step 1) described in coenzyme Q10, obtained by following steps:
1. pre-treatment: by waste/hypo-tobacco leaf through extracting the tobacco leaf extract obtained, add equivalent weight
Pure water, puts into high speed dispersion mulser and processes, and rotating speed 2500r/min, time 8min obtain height
Speed dispersion and emulsion thing, then use ethanol solution and the petroleum ether system dynamic saponification combined state eggplant of NaOH
Buddhist nun's alcohol, crystallizes, filters, and obtains the extractum containing Salanesol；
2. molecular distillation: the extractum containing Salanesol step 1. obtained, is removed by molecular distillation
Miscellaneous, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3. pillar layer separation: the heavy phase Salanesol acetone solution that step 2. obtained, filtration is logical
Cross pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize deionization
Water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4. the preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5. the molecular distillation that 3. the light phase Salanesol that step 2. obtained, step obtain purify after eggplant
The methyl dimethoxy epoxide benzoquinone that 4. Buddhist nun's alcohol and step obtain mixes with the weight ratio of 2.5:70:1.5,
Reaction obtains coenzyme Q10.
Step 1 of the present invention) described in coenzyme Q10, gelatin substance, saccharide, emulsifying agent, solvable
Property starch, cosolvent, preferably according to 1:0.20-0.30:0.02-0.04:0.004-0.006:
0.04-0.06:0.02-0.04 weight ratio, described water meets prior art regulation.
Step 1) described in gelatin substance, preferably arabic gum and gelatin；
Described sugar, preferably lactose, D-galactose；
Described emulsifying agent, preferably tween, sucrose ester；
Described cosolvent, preferably Polyethylene Glycol, poloxamer.
Step 2) and step 3) described in heating for dissolving, preferred 55-60 DEG C of temperature.
The invention still further relates to the coenzyme Q10 using above-mentioned preparation method to obtain, medically can be used for painstaking effort
Guard system disease, can be widely used for the industries such as food, cosmetics, dietary supplement, has raising people
The functions such as body immunity, enhancing antioxidation, slow down aging and enhancing human activity.
Compared with prior art, advantages of the present invention:
1, current, food or the high pressure of health food or ultra high pressure treatment, be at the high pressure sealed
Or in ultrahigh pressure vessel, as medium, food is applied with liquid (mainly water) pressure of hundreds of MPas
Power processes, and under high pressure, the macromolecular structure material such as protein in food, starch becomes
Changing, its result is protein denaturation, starch gelatinization, enzyme inactivation, microorganism death, with heat treated
Technique is compared, and HIGH PRESSURE TREATMENT maximum is advantageous in that, it to the flavor substance of food, vitamin,
The not impact such as pigment, nutrition loss is little, but the pressure of HIGH PRESSURE TREATMENT is bigger just can be reached
To effect.The present invention is by " being forced into 4kg/cm2So that it is pressure is uniform, and keeps 10-15min,
Then in 1-3s, recover normal pressure ", the pressure of employing is far smaller than the pressure used by existing high pressure technique,
And by moment, pressure is reduced to 0, so that aqueous phase and oil phase dissolve each other, compared to existing technology,
Effective, the time is short.
2, the present invention keeps 10-15min pressing time, and pressing time is short, and pressure is little, does not destroy product
The biological activity of product, product stability is good, and without organic solvent in preparation process, safety is high,
Green, environmental protection.
3, the coenzyme Q10 content that prior art obtains is usually no more than 98%, and color and luster is dim, and this
The coenzyme Q10 content that invention obtains is more than 98%, and has higher color valency, bright color, system
Standby aqueous dispersion, color and luster is good, and in application, adaptability is wider, and because color valency is high, content is high,
So the application cost of corresponding aqueous dispersion can reduce.
Detailed description of the invention
With embodiment, the invention will be further described below, but the invention is not limited in that these are implemented
Example.
Embodiment 1:
A kind of coenzyme Q10 aqueous dispersion and preparation method thereof, specifically includes following steps:
1) raw material prepares: according to the weight ratio of 1:0.20:0.04:0.004:0.06:0.02,
Prepare coenzyme Q10, arabic gum, lactose, emulsifying agent, soluble starch, cosolvent, Yi Jishui；
2) arabic gum is dissolved in water, adds soluble starch, lactose, tween, heat 55 DEG C
Dissolve, stir, standby；
3) by Polyethylene Glycol heating for dissolving, add coenzyme Q10, heat 55 DEG C of dissolvings, standby；
4) pressurized treatments: by step 2) and step 3) process after material, put in pressure pan,
It is forced into 4kg/cm2So that it is pressure is uniform, and keeps 5-10min, then often recovers in 1-3s
Pressure, obtains mixed liquor；
5) by step 4) mixed liquor that obtains is spray-dried, and obtains coenzyme Q10 aqueous dispersion powder；
Step 1) described in coenzyme Q10, obtained by following steps:
1. pre-treatment: by waste/hypo-tobacco leaf through extracting the tobacco leaf extract obtained, add equivalent weight
Pure water, puts into high speed dispersion mulser and processes, and rotating speed 2500r/min, time 8min obtain height
Speed dispersion and emulsion thing, then use ethanol solution and the petroleum ether system dynamic saponification combined state eggplant of NaOH
Buddhist nun's alcohol, crystallizes, filters, and obtains the extractum containing Salanesol；
2. molecular distillation: the extractum containing Salanesol step 1. obtained, is removed by molecular distillation
Miscellaneous, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3. pillar layer separation: the heavy phase Salanesol acetone solution that step 2. obtained, filtration is logical
Cross pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize deionization
Water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4. the preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5. the molecular distillation that 3. the light phase Salanesol that step 2. obtained, step obtain purify after eggplant
The methyl dimethoxy epoxide benzoquinone that 4. Buddhist nun's alcohol and step obtain mixes with the weight ratio of 2.5:70:1.5,
Reaction obtains coenzyme Q10.
Embodiment 2:
A kind of coenzyme Q10 aqueous dispersion and preparation method thereof, specifically includes following steps:
1) raw material prepares: according to the weight ratio of 1:0.30:0.02:0.006:0.04:0.04,
Prepare coenzyme Q10, gelatin, D-galactose, emulsifying agent, soluble starch, cosolvent, Yi Jishui；
2) gelatin is dissolved in water, adds soluble starch, D-galactose, tween, heat 60 DEG C
Dissolve, stir, standby；
3) by Polyethylene Glycol heating for dissolving, add coenzyme Q10, heat 60 DEG C of dissolvings, standby；
4) pressurized treatments: by step 2) and step 3) process after material, put in pressure pan,
It is forced into 4kg/cm2So that it is pressure is uniform, and keeps 5-10min, then often recovers in 1-3s
Pressure, obtains mixed liquor；
5) by step 4) mixed liquor that obtains is spray-dried, and obtains coenzyme Q10 aqueous dispersion powder；
Step 1) described in coenzyme Q10, obtained by following steps:
1. pre-treatment: by waste/hypo-tobacco leaf through extracting the tobacco leaf extract obtained, add equivalent weight
Pure water, puts into high speed dispersion mulser and processes, and rotating speed 2500r/min, time 8min obtain height
Speed dispersion and emulsion thing, then use ethanol solution and the petroleum ether system dynamic saponification combined state eggplant of NaOH
Buddhist nun's alcohol, crystallizes, filters, and obtains the extractum containing Salanesol；
2. molecular distillation: the extractum containing Salanesol step 1. obtained, is removed by molecular distillation
Miscellaneous, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3. pillar layer separation: the heavy phase Salanesol acetone solution that step 2. obtained, filtration is logical
Cross pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize deionization
Water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4. the preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5. the molecular distillation that 3. the light phase Salanesol that step 2. obtained, step obtain purify after eggplant
The methyl dimethoxy epoxide benzoquinone that 4. Buddhist nun's alcohol and step obtain mixes with the weight ratio of 2.5:70:1.5,
Reaction obtains coenzyme Q10.
Embodiment 3:
A kind of coenzyme Q10 aqueous dispersion and preparation method thereof, specifically includes following steps:
1) raw material prepares: according to the weight ratio of 1:0.25:0.03:0.005:0.05:0.03,
Prepare coenzyme Q10, arabic gum, lactose, emulsifying agent, soluble starch, cosolvent, Yi Jishui；
2) arabic gum is dissolved in water, adds soluble starch, lactose, sucrose ester, heating
55 DEG C of dissolvings, stir, standby；
3) by poloxamer heating for dissolving, add coenzyme Q10, heat 60 DEG C of dissolvings, standby；
4) pressurized treatments: by step 2) and step 3) process after material, put in pressure pan,
It is forced into 4kg/cm2So that it is pressure is uniform, and keeps 5-10min, then often recovers in 1-3s
Pressure, obtains mixed liquor；
5) by step 4) mixed liquor that obtains is spray-dried, and obtains coenzyme Q10 aqueous dispersion powder；
Step 1) described in coenzyme Q10, obtained by following steps:
1. pre-treatment: by waste/hypo-tobacco leaf through extracting the tobacco leaf extract obtained, add equivalent weight
Pure water, puts into high speed dispersion mulser and processes, and rotating speed 2500r/min, time 8min obtain height
Speed dispersion and emulsion thing, then use ethanol solution and the petroleum ether system dynamic saponification combined state eggplant of NaOH
Buddhist nun's alcohol, crystallizes, filters, and obtains the extractum containing Salanesol；
2. molecular distillation: the extractum containing Salanesol step 1. obtained, is removed by molecular distillation
Miscellaneous, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3. pillar layer separation: the heavy phase Salanesol acetone solution that step 2. obtained, filtration is logical
Cross pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize deionization
Water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4. the preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5. the molecular distillation that 3. the light phase Salanesol that step 2. obtained, step obtain purify after eggplant
The methyl dimethoxy epoxide benzoquinone that 4. Buddhist nun's alcohol and step obtain mixes with the weight ratio of 2.5:70:1.5,
Reaction obtains coenzyme Q10.
The coenzyme Q10 that different preparation methoies obtain:
Comparative example 1:
1) pre-treatment: by waste/hypo-tobacco leaf through extracting the tobacco leaf extract obtained, use the ethanol of NaOH
Solution and petroleum ether system dynamic saponification combined state Salanesol, crystallize, filter, obtain containing Salanesol
Extractum；
2) molecular distillation: by step 1) extractum containing Salanesol that obtains, passes through molecular distillation
Remove impurity, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3) pillar layer separation: by step 2) obtain heavy phase Salanesol acetone solution, filtration,
By pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize go from
Sub-water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4) preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5) by step 2) the light phase Salanesol that obtains, step 3) after the molecular distillation that obtains purifies
Salanesol and step 4) the methyl dimethoxy epoxide benzoquinone that obtains mixes with the weight ratio of 2.5:70:1.5
Closing, reaction obtains coenzyme Q10.
Comparative example 2:
A kind of method extracting coenzyme Q10 from Nicotiana tabacum L., specifically includes following steps:
1) pre-treatment: smashed by waste/hypo-tobacco leaf, adds the pure water of equivalent weight, puts into and divides at a high speed
Dissipate mulser to process, rotating speed 2500r/min, time 8min, obtain high speed dispersion emulsion, pass through
Extract the tobacco leaf extract obtained, then use ethanol solution and the petroleum ether system dynamic saponification knot of NaOH
Close state Salanesol, crystallize, filter, obtain the extractum containing Salanesol；
2) molecular distillation: by step 1) extractum containing Salanesol that obtains, passes through molecular distillation
Remove impurity, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3) pillar layer separation: by step 2) obtain heavy phase Salanesol acetone solution, filtration,
By pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize go from
Sub-water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4) preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5) by step 2) the light phase Salanesol that obtains, step 3) after the molecular distillation that obtains purifies
Salanesol and step 4) the methyl dimethoxy epoxide benzoquinone that obtains mixes with the weight ratio of 2.5:70:1.5
Closing, reaction obtains coenzyme Q10.
Color valency is tested:
1, main operational steps: the coenzyme Q10 sample 0.00266g in accurate weighing embodiment 3,
Put in 10ml volumetric flask, dissolve with distilled water, ultrasonic 5min, treat that sample solution is cooled to room
Wen Hou, with distilled water constant volume to 10ml, takes in the cuvette that 4ml testing sample solution transfers to 1cm,
To be checked.Using spectrophotometer to detect sample solution, testing conditions is: detection wavelength:
440nm；Temperature: room temperature；Return to zero with distilled water, then sample is detected.
2, calculate:
Detect that A value is 2.3679；2.3679；
A value exceeds 0.2000-0.6000 scope, so needing to take out sample solution 1ml more fixed
Holding in 10ml volumetric flask, i.e. dilution 10 times, repeats above-mentioned detecting step, detects that A value is
0.2951；0.2962；0.2966；0.2967.
Experimental data substitutes into above-mentioned formula obtain:
CalculateIt is respectively as follows: 110；111；111；111.
Error amount < 2%.
Iu converts: 111*100,000/150=74000ICU.
3, result: embodiment 3 sample color valency is 111, international color is worth as 74000ICU.
Result:
Claims (7)
1. coenzyme Q10 aqueous dispersion and preparation method thereof, it is characterised in that include walking as follows
Rapid:
1) raw material prepares: get out coenzyme Q10, gelatin substance, sugar, emulsifying agent, solubility shallow lake
Powder, cosolvent, water；
2) gelatin substance is dissolved in water, adds soluble starch, saccharide, emulsifying agent, heating
Dissolve, stir, standby；
3) by cosolvent heating for dissolving, coenzyme Q10 is added, heating for dissolving, standby；
4) pressurized treatments: by step 2) and step 3) process after material, put in pressure pan,
It is forced into 4kg/cm2So that it is pressure is uniform, and keeps 5-10min, then often recovers in 1-3s
Pressure, obtains mixed liquor；
5) by step 4) mixed liquor that obtains is spray-dried, and obtains coenzyme Q10 aqueous dispersion powder；
Step 1) described in coenzyme Q10, obtained by following steps:
1. pre-treatment: by waste/hypo-tobacco leaf through extracting the tobacco leaf extract obtained, add equivalent weight
Pure water, puts into high speed dispersion mulser and processes, and rotating speed 2500r/min, time 8min obtain height
Speed dispersion and emulsion thing, then use ethanol solution and the petroleum ether system dynamic saponification combined state eggplant of NaOH
Buddhist nun's alcohol, crystallizes, filters, and obtains the extractum containing Salanesol；
2. molecular distillation: the extractum containing Salanesol step 1. obtained, is removed by molecular distillation
Miscellaneous, vacuum 0.01Pa, vapo(u)rizing temperature 190 DEG C, scraper plate rotating speed 600r/min, mass flow
1.0mL/min, obtains light phase Salanesol and heavy phase Salanesol；
3. pillar layer separation: the heavy phase Salanesol acetone solution that step 2. obtained, filtration is logical
Cross pillar layer separation, use ZTC-1 macroporous adsorbent resin, flow velocity be 2 seconds 3, utilize deionization
Water and 20%, 30%, 40%, 50%, 95% ethanol (v/v) carry out gradient elution, collect eluent,
Concentrate, obtain the Salanesol after molecular distillation purifies；
4. the preparation of methyl dimethoxy epoxide benzoquinone: methylphenol is obtained by bromo etherification oxidation
Methyl dimethoxy epoxide benzoquinone；
5. the molecular distillation that 3. the light phase Salanesol that step 2. obtained, step obtain purify after eggplant
The methyl dimethoxy epoxide benzoquinone that 4. Buddhist nun's alcohol and step obtain mixes with the weight ratio of 2.5: 70: 1.5,
Reaction obtains coenzyme Q10.
A kind of coenzyme Q10 aqueous dispersion the most according to claim 1 and preparation method thereof, its
Be characterised by: step 1) described in coenzyme Q10, gelatin substance, saccharide, emulsifying agent, solvable
Property starch, cosolvent, according to 1:0.20-0.30:0.02-0.04:0.004-0.006:
0.04-0.06:0.02-0.04 weight ratio.
A kind of coenzyme Q10 aqueous dispersion the most according to claim 1 and preparation method thereof, its
Be characterised by: step 1) described in gelatin substance, for arabic gum and gelatin.
A kind of coenzyme Q10 aqueous dispersion the most according to claim 1 and preparation method thereof, its
Be characterised by: step 1) described in sugar, for lactose, D-galactose.
A kind of coenzyme Q10 aqueous dispersion the most according to claim 1 and preparation method thereof, its
Be characterised by: step 1) described in emulsifying agent, for tween, sucrose ester.
A kind of coenzyme Q10 aqueous dispersion the most according to claim 1 and preparation method thereof, its
Be characterised by: step 1) described in cosolvent, for Polyethylene Glycol, poloxamer.
A kind of coenzyme Q10 aqueous dispersion the most according to claim 1 and preparation method thereof, its
Be characterised by: step 2) and step 3) described in heating for dissolving, temperature is 55-60 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020156302A1 (en) * | 2001-04-19 | 2002-10-24 | West Daniel David | Synthesis of coenzyme Q10, ubiquinone |
| CN1951888A (en) * | 2005-10-22 | 2007-04-25 | 郑亚津 | Process for purifying solanesol from tobacco leaf extract |
| CN101288641A (en) * | 2007-04-19 | 2008-10-22 | 浙江一新制药股份有限公司 | Coenzyme Q10 water dispersion and preparation method thereof |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020156302A1 (en) * | 2001-04-19 | 2002-10-24 | West Daniel David | Synthesis of coenzyme Q10, ubiquinone |
| CN1951888A (en) * | 2005-10-22 | 2007-04-25 | 郑亚津 | Process for purifying solanesol from tobacco leaf extract |
| CN101288641A (en) * | 2007-04-19 | 2008-10-22 | 浙江一新制药股份有限公司 | Coenzyme Q10 water dispersion and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 辛秀兰: "《现代生物制药工艺学》", 31 August 2006, 化学工业出版社 * |
| 邸羿等: "高剪切分散乳化技术提取茶叶中有效成分的动力学及热力学研究", 《分析测试学报》 * |
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