CN114028446A - 一种蓝莓口服液及其制备方法 - Google Patents
一种蓝莓口服液及其制备方法 Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/45—Ericaceae or Vacciniaceae (Heath or Blueberry family), e.g. blueberry, cranberry or bilberry
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/46—Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
- A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Organic Chemistry (AREA)
- Epidemiology (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Biochemistry (AREA)
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- Alternative & Traditional Medicine (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
本发明公开了一种蓝莓口服液的制备方法,取品种为蓝雨的蓝莓冻果冷冻干燥制成蓝莓果渣粉,蓝莓果渣粉用含1%柠檬酸的50%乙醇,超声波细胞破碎机提取处理,得到花青素粗提液冷冻干燥,得到冻干粗滤物;冻干粗滤物经大孔树脂吸附后,再用蒸馏水、含3%柠檬酸的60%乙醇洗脱,得到花青素浓缩液备用;取蓝莓果汁静置24h后的上层澄清液与花青素浓缩液、蜂蜜、抗坏血酸混合,即得一种蓝莓口服液。本发明所采用的工艺均为全程低温,最大限度保留花青素,减少降解,保持活性,保证了口服液中的花青素含量以及抗氧化效果;同时在提取花青素耗时短,效用高。采用果汁和花青素浓缩液复配的工艺,为口服液提供了天然蓝莓的风味,口感更佳。
Description
技术领域
本发明属于医药技术领域,尤其涉及一种蓝莓口服液的制备方法以及采用该制备方法制得的蓝莓口服液。
背景技术
蓝莓(Blueberry)为杜鹃花科(Ericaceae)越桔属(Vaccinium spp)的多年生常绿或落叶灌木,果实几乎是圆形、蓝色或紫色的小浆果,又称为越橘、蓝浆果等,酸甜度适宜,其果肉细腻且皮薄种籽小。蓝莓果实含有丰富的营养成分。在越橘属植物种类中蓝莓是营养成分含量最多的一种,除含丰富的的有机酸和糖外,还含有大量种类的其他营养成分,如超氧化物歧化酶(SOD)、不饱和脂肪酸、矿物质和多种维生素等,以及黄酮、花青素、尼克酸等特殊成分。孟宪军等研究表明:蓝莓果实对保护视力、延缓衰老和抗癌等有奇特的功效。蓝莓还被***粮农组织(FAO)确定为人类五大健康食品之一。因此,蓝莓除鲜食外,还被大量加工成为食品、保健品、药品、休闲食品等,深受消费者喜爱。
蓝莓中花青素的含量是目前所有果蔬中花青素含量最高的。有研究分析测定了100g蓝莓冻果中蓝莓花青素的含量在327.35mg左右。花青素是一种有效的天然游离基消除剂,其消除效果是L-抗坏血酸的20倍,是维生素E的50倍,花青素在自然条件下不稳定,通常以糖苷键的形式与糖分子结合形成相对稳定的花色苷。蓝莓花青素具有很好的保健作用,如抗氧化功能、抗癌、自由基的清除和保护视力等。李颖畅等研究发现蓝莓花色苷能有效清楚超氧阴离子和羟基自由基以及抗脂质体过氧化等。
目前市售蓝莓保健品中大多都以花青素及其功效为主,备受消费者青睐,且售价昂贵。产品包括有蓝莓花青素咀嚼片、蓝莓花青素护眼胶囊、蓝莓叶黄素酯咀嚼片等。此类产品皆因蓝莓花青素具有促进视紫质再生,改善视力,抗疲劳等对视力的保护作用;是天然水溶性自由基清除剂,具有抗脂质体过氧化,清除羟基自由基和超氧阴离子自由基的能力以及调节血管收缩,维持正常的血压范围,保护血管,强力持续毛细管的参透性等功能作用。
CN201610160610.7公开了一种纯天然的蓝莓花青素苷元口服液及制备方法,其采用了溶剂萃取及层析联用技术,在简化操作工艺及节约成本的基础上,制得了纯天然、易吸收的花青素苷元口服液,具有较高营养价值和保健功能,适用人群广泛。但该技术在对花青素提纯时采用了低毒性的乙酸乙酯,存在残留风险,此外提取花青素的时间较长,在后续灭菌过程中,采用UHT灭菌,灭菌温度高,花青素降解严重。CN201611080148.6公开了一种改善视力的蓝莓花青素口服液及其制备方法,将蓝莓花青素浓缩液,蓝莓原果汁,抗坏血酸,乳酸锌,木糖醇,置于配料罐中,加总体积1/5的去离子水在35℃使其充分溶解,定容至容器刻度,搅拌充分溶解后,过滤、混匀灌装,封口,杀菌,灯检,包装,检验合格后即得成品。该发明在制备过程中农花青素没有经过纯化,纯度低,制得的成品中花青素含量较低,此外灭菌温度高,花青素大量降解导致活性下降。
基于上述分析,一种花青素含量高、最大程度保留其活性,花青素提取时间短、提取过程中不存在化学残留的蓝莓口服液是目前行业内急需的。
发明内容
鉴于上述不足,本发明提供了一种花青素含量高的蓝莓口服液及其制备方法,不仅能最大限度保留花青素抗氧化活性,同时生产过程中不存在化学残留,花青素提取时间明显缩短,效率得到有效提升。
本发明是通过如下手段实现的:
一种蓝莓口服液的制备方法,包括:
(1)选取花青素含量高的蓝莓品种蓝雨的冻果,解冻清洗后榨汁,过滤,分离蓝莓果汁和果渣,将果渣冷冻干燥后超微粉碎,得到蓝莓果渣粉备用;
(2)取蓝莓果渣粉以1:20的比例加入含1%柠檬酸的50%乙醇,用超声波细胞破碎机以225W功率超声提取20分钟,过滤,取滤液低温旋转蒸发回收乙醇,得到花青素粗提液,将粗提液冷冻干燥,得到冻干粗滤物备用;
(3)将冻干粗滤物用含3%柠檬酸的蒸馏水溶解,用大孔树脂纯化,上样速度2倍柱体积每小时,依次用蒸馏水、含3%柠檬酸的60%乙醇洗脱,收集乙醇洗脱液,40℃旋转蒸发至原体积的5-10%,回收乙醇,得到花青素浓缩液备用;
(4)果步骤(1)得到的蓝莓果汁静置24小时,取上层澄清液,得到澄清果汁备用;
(5)取澄清果汁40份,花青素浓缩液50份,蜂蜜10份,抗坏血酸0.05份混合,均质,采用0.2-0.4μm滤膜过滤、除菌,罐装,即得一种蓝莓口服液。
本发明的有益效果在于:
本发明所采用的工艺均为全程低温,最大限度保留花青素,减少降解,保持活性,保证了口服液中的花青素含量以及抗氧化效果;同时在提取花青素耗时短,效用高。采用果汁和花青素浓缩液复配的工艺,为口服液提供了天然蓝莓的风味,口感更佳。
具体实施方式
下面将结合本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种蓝莓口服液的制备方法,包括:
(1)选取花青素含量高的蓝莓品种蓝雨的冻果,解冻清洗后榨汁,过滤,分离蓝莓果汁和果渣,将果渣冷冻干燥后超微粉碎,得到蓝莓果渣粉备用;
(2)取蓝莓果渣粉以1:20的比例加入含1%柠檬酸的50%乙醇,用超声波细胞破碎机以225W功率超声提取20分钟,过滤,取滤液低温旋转蒸发回收乙醇,得到花青素粗提液,将粗提液冷冻干燥,得到冻干粗滤物备用;
(3)将冻干粗滤物用含3%柠檬酸的蒸馏水溶解,用大孔树脂纯化,上样速度2倍柱体积每小时,依次用蒸馏水、含3%柠檬酸的60%乙醇洗脱,收集乙醇洗脱液,40℃旋转蒸发至原体积的7.5%,回收乙醇,得到花青素浓缩液备用;
(4)蓝莓果汁静置24小时,除去下层果肉,得到澄清果汁备用;
(5)取澄清果汁40份,花青素浓缩液50份,蜂蜜10份,抗坏血酸0.05份混合,均质,采用0.3μm滤膜过滤、除菌,罐装,即得一种蓝莓口服液。
实施例2
一种蓝莓口服液的制备方法,包括:
(1)选取花青素含量高的蓝莓品种蓝雨的冻果,解冻清洗后榨汁,过滤,分离蓝莓果汁和果渣,将果渣冷冻干燥后超微粉碎,得到蓝莓果渣粉备用;
(2)取蓝莓果渣粉以1:20的比例加入含1%柠檬酸的50%乙醇,用超声波细胞破碎机以225W功率超声提取20分钟,过滤,取滤液低温旋转蒸发回收乙醇,得到花青素粗提液,将粗提液冷冻干燥,得到冻干粗滤物备用;
(3)将冻干粗滤物用含3%柠檬酸的蒸馏水溶解,用大孔树脂纯化,上样速度2倍柱体积每小时,依次用蒸馏水、含3%柠檬酸的60%乙醇洗脱,收集乙醇洗脱液,40℃旋转蒸发至原体积的5%,回收乙醇,得到花青素浓缩液备用;
(4)蓝莓果汁静置24小时,除去下层果肉,得到澄清果汁备用;
(5)取澄清果汁40份,花青素浓缩液50份,蜂蜜10份,抗坏血酸0.05份混合,均质,采用0.2μm滤膜过滤、除菌,罐装,即得一种蓝莓口服液。
实施例3
一种蓝莓口服液的制备方法,包括:
(1)选取花青素含量高的蓝莓品种蓝雨的冻果,解冻清洗后榨汁,过滤,分离蓝莓果汁和果渣,将果渣冷冻干燥后超微粉碎,得到蓝莓果渣粉备用;
(2)取蓝莓果渣粉以1:20的比例加入含1%柠檬酸的50%乙醇,用超声波细胞破碎机以225W功率超声提取20分钟,过滤,取滤液低温旋转蒸发回收乙醇,得到花青素粗提液,将粗提液冷冻干燥,得到冻干粗滤物备用;
(3)将冻干粗滤物用含3%柠檬酸的蒸馏水溶解,用大孔树脂纯化,上样速度2倍柱体积每小时,依次用蒸馏水、含3%柠檬酸的60%乙醇洗脱,收集乙醇洗脱液,40℃旋转蒸发至原体积的10%,回收乙醇,得到花青素浓缩液备用;
(4)蓝莓果汁静置24小时,除去下层果肉,得到澄清果汁备用;
(5)取澄清果汁40份,花青素浓缩液50份,蜂蜜10份,抗坏血酸0.05份混合,均质,采用0.4μm滤膜过滤、除菌,罐装,即得一种蓝莓口服液。
对比例1
采用CN201610160610.7公开的相关工艺制取一种纯天然的蓝莓花青素苷元口服液。
对比例2
采用CN201611080148.6公开的相关工艺制取一种改善视力的蓝莓花青素口服液。
试验例1
经高效液相色谱测定实施例1~3、对比例1~2所得样品中的花青素的含量与活性。具体结果详见表1:
表1
分组 | 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 |
花青素含量 | 15.1% | 12.2% | 11.3% | 3.2% | 0.5% |
根据表1结果可知,本发明工艺制得的蓝莓口服液中花青素含量高达11.3%以上,以实施例1中制得的口服液含量花青素最高,为15.1%;三组实施例花青素含量均显著高于两组对照组的花青素含量,由此证明,本发明工艺制得的口服液能有效提升花青素的含量。
试验例2
测定实施例1~3、对比例1~2所得样品的抗氧化效果。
总还原能力的测定
测定方法
移取1mL不同浓度样品于试管中,然后加入1mL 0.2mol/L磷酸钠缓冲液(pH=6.6),然后加入1mL的铁***溶液,混匀后在50℃条件下培养20min,接着冷却加入1mL10%三氯乙酸溶液定容至10mL,4000rmp/min离心8min,移取2.5mL上清液于5mL容量瓶中,加入0.5mL0.1%三氯化铁溶液,快速摇匀定容至5mL,室温静置10min,在700nm处测定吸光值,对照组用无水乙醇代替样品溶液,每个样品做三次平行实验,取平均数。具体结果详见表1:
表2
分组 | 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 |
总还原能力 | 78.25 | 70.16 | 75.84 | 25.69 | 32.15 |
根据表2结果可知,本发明工艺制得的蓝莓口服液的总还原能力达到70以上,以实施例1中制得的口服液的总还原能力最高,为78.25;三组实施例花青素含量均显著高于两组对照组的花青素含量,由此证明,本发明工艺制得的口服液具有显著的抗氧化效果。
综上所述,本发明所采用的工艺均为全程低温,最大限度保留花青素,减少降解,保持活性,保证了口服液中的花青素含量以及抗氧化效果;同时在提取花青素耗时短,效用高。
需要说明的是,在本文中,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种蓝莓口服液,包括:
蓝莓果汁40份;
花青素浓缩液50份;
蜂蜜10份;
以及抗坏血酸0.05份;
其中蓝莓果汁为静置后去除果肉的上层澄清果汁。
2.一种制备如权利要求1所述蓝莓口服液的方法,包括:
取蓝莓果汁、花青素浓缩液、蜂蜜、抗坏血酸混合均质;
采用0.2-0.4μm滤膜过滤、除菌;
罐装,即得一种蓝莓口服液。
3.根据权利要求2所述的制备方法,其中:
所述蓝莓果汁由如下方法制得:
取品种为蓝雨的蓝莓冻果,解冻榨汁;
过滤果渣得到果汁;
果汁静置24小时,取上层澄清液,即得。
4.根据权利要求2所述的制备方法,其中:
所述花青素浓缩液由如下方法制得:
取品种为蓝雨的蓝莓冻果,解冻榨汁,过滤后分离出果渣备用;
果渣冷冻干燥后进行超微粉碎,得到蓝莓果渣粉备用;
蓝莓果渣粉经50%的乙醇进行超声波细胞破碎机提取,过滤得到滤液;
滤液经低温旋转蒸发后收集乙醇,得到粗提液;
粗提液经冷冻干燥后,得到冻干粗滤物;
冻干粗滤物经蒸馏水溶解后,辅以大孔树脂纯化;
随后洗脱,收集乙醇洗脱液;
将乙醇洗脱液经旋转蒸发,回收乙醇,即得花青素浓缩液。
5.根据权利要求4所述的制备方法,其中:
所述果渣粉与50%的乙醇的料液比为1:20(m/υ);
所述50%的乙醇中还含有1%的柠檬酸。
6.根据权利要求4所述的制备方法,其中:
所述超声细胞破碎机的提取功率为225w,提取时间为20min。
7.根据权利要求4所述的制备方法,其中:
所述溶解冻干粗滤物的蒸馏水中还包括3%的柠檬酸;
所述大孔树脂纯化的上样速度为2倍柱体积每小时。
8.根据权利要求4所述的制备方法,其中:
所述洗脱依次采用蒸馏水以及含3%柠檬酸的60%乙醇。
9.根据权利要求4所述的制备方法,其中:
所述旋转蒸发温度为40℃,蒸发至原体积的5%~10%。
10.一种根据权利要求2~9所述任一制备方法制得的蓝莓口服液。
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CN106539086A (zh) * | 2016-11-30 | 2017-03-29 | 贵阳学院 | 一种改善视力的蓝莓花青素口服液及其制备方法 |
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CN105708795A (zh) * | 2016-03-21 | 2016-06-29 | 吉林大学 | 一种纯天然的蓝莓花青素苷元口服液及制备方法 |
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