CN105748350A - 一种包覆型自由基清除剂的制备方法 - Google Patents
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Abstract
本发明公开了一种包覆型自由基清除剂的制备方法,属于自由基清除剂领域。本发明分别从银杏果和人参茎叶中提取出自由基清除剂并混合,再利用蓖麻油和壳聚糖形成的油糖混合粘稠液包覆在自由基清除剂表面,最后通过真空冻干、粉碎即可,本发明利用蓖麻油和壳聚糖形成的粘稠物包覆在自由基清除剂表面,形成一层稳定的保护层,有效防止自由基清除剂被氧化,提高其活性,使其具有更强的抗氧化性能,而且原料丰富,制备成本低。
Description
技术领域
本发明公开了一种包覆型自由基清除剂的制备方法,属于自由基清除剂领域。
背景技术
自由基是人体正常的代谢产物,正常情况下人体内自由基是处于不断产生与清除的动态平衡中。人体内存在少量的氧自由基,不但对人体不构成威胁,而且可以促进细胞增殖,刺激白细胞和吞噬细胞杀灭细菌,消除炎症,分解毒物.但如果人体内氧自由基的数量过多,就会破坏细胞结构,引起脂质过氧化,干扰人体的正常代谢活动,引起疾病,加速人体衰老进程。
自由基清除剂是指能清除自由基或能阻断自由基参与的氧化反应的物质。自由基清除剂可分为酶类清除剂和非酶类清除剂两大类.酶类清除剂一般为抗氧化酶,主要有超氧化物歧化酶、过氧化氢酶和谷胱甘肽过氧化酶。非酶类自由基清除剂一般是一些抗氧化剂,如维生素E、维生素A、β-胡萝卜素、茶多酚、黄酮化合物和还原型谷胱甘肽等。
银杏是一种重要的经济作物,有着重要的药用价值。银杏叶提取物具有直接清除氧自由基的能力已被证实。银杏树的果实(白果)含丰富的植物蛋白、糖份、苷类等多种生物活性物质,是传统的滋补食物和药物。白果同样可以提取具有超氧自由基清除能力的活性物质。
人参是传统的名贵中药具有极高药用价值。人参提取物中含有皂甙、多糖及挥发油等多种化学成份。其中人参皂甙为人参的主要药用有效成份,具有抑制血小板聚集、清除超氧阴离子自由基等作用。
发明内容
本发明主要解决的技术问题:针对目前发现的天然抗氧化剂,成本较高,提取工艺复杂,得到的自由基清除剂性质不稳定,易被氧化,从银杏中得到的自由基清除剂活性极低,很容易失活的问题,提供了一种包覆型自由基清除剂的制备方法,本发明分别从银杏果和人参茎叶中提取出自由基清除剂并混合,再利用蓖麻油和壳聚糖形成的油糖混合粘稠液包覆在自由基清除剂表面,最后通过真空冻干、粉碎即可,本发明利用蓖麻油和壳聚糖形成的粘稠物包覆在自由基清除剂表面,形成一层稳定的保护层,有效防止自由基清除剂被氧化,提高其活性,使其具有更强的抗氧化性能,而且原料丰富,制备成本低。
为了解决上述技术问题,本发明所采用的技术方案是:
(1)取1~2kg新鲜银杏果剥除果肉外层硬壳,将除壳后的银杏果和蒸馏水按体积比1:1进行混合后放入匀浆机中破碎匀浆,量取200~250mL破碎后的银杏果匀浆装入1L烧杯中,再向烧杯中加入匀浆体积2~3倍pH为7.6的磷酸盐缓冲液,用玻璃棒搅拌均匀;
(2)将上述搅拌均匀后的混合液移入索式抽提器中抽提3~5h,量取300~400mL抽提液和100~150mL浓度0.5mol/L硫酸铵溶液放置在磁力搅拌机上搅拌均匀后移入冰水浴中,在4~6℃下静置沉淀过夜,再用卧式离心机以5000~7000r/min转速离心分离得到上清液;
(3)将上述得到的上清液装入透析袋中,以1~2L流动的无水乙醇作为透析液,对上清液进行循环透析12~15h,收集循环透析后的无水乙醇放在旋转蒸发器中,在60~70℃下旋蒸浓缩至原体积的1/10,得到浓缩银杏果提取物,备用;
(4)称取400~500g人参茎叶放入气流粉碎机粉碎后按固液比为1:3将茎叶粉末和正丁醇混合,混合后倒入超声萃取仪中,在100~200W功率下超声萃取1~2h,过滤分离得到萃取液,将所得萃取液过大孔吸附树脂柱,再用大孔吸附树脂体积5~8倍的质量浓度75%无水乙醇对吸附树脂进行洗脱并收集洗脱液;
(5)将上述收集到的洗脱液放入蒸馏装置中,在60~70℃下蒸馏回收乙醇,得到人参皂甙,将100~200mL人参皂甙和200~300mL备用的浓缩银杏果提取物进行混合,得混合自由基清除剂粗品,放在棕色瓶中保存;
(6)量取100~200mL蓖麻油放入铁锅中,加热升温至100~110℃后,向油中加入10~20g壳聚糖,用铁勺不断搅拌,直至壳聚糖完全溶解,油糖混合液变粘稠后,使其自然冷却至室温,再加入等体积上述清除剂粗品混合均匀后,放入真空冻干机冻干后粉碎并过100目标准筛得粉末,包装后,即得一种包覆型自由基清除剂。
所述的步骤(4)中大孔树脂为D101型大孔吸附树脂。
本发明的应用的方法:本发明制备得到的自由基清除剂可以添加到保健品、化妆品和医药中,也可以作为食品添加保护剂,人体从膳食中补充自由基清除剂,从而达到防御疾病、延缓衰老的目的。
本发明的有益效果是:
(1)本发明利用蓖麻油和壳聚糖形成的粘稠物包覆在自由基清除剂表面,形成一层稳定的保护层,有效防止其被氧化,提高活性,具有更强的抗氧化性能;
(2)本发明采用的蓖麻油和壳聚糖为包覆材料,安全环保,食用安全;
(3)而且制备工艺简单,成本低。
具体实施方式
首先取1~2kg新鲜银杏果剥除果肉外层硬壳,将除壳后的银杏果和蒸馏水按体积比1:1进行混合后放入匀浆机中破碎匀浆,量取200~250mL破碎后的银杏果匀浆装入1L烧杯中,再向烧杯中加入匀浆体积2~3倍pH为7.6的磷酸盐缓冲液,用玻璃棒搅拌均匀;搅拌均匀后的混合液移入索式抽提器中抽提3~5h,量取300~400mL抽提液和100~150mL浓度0.5mol/L硫酸铵溶液放置在磁力搅拌机上搅拌均匀后移入冰水浴中,在4~6℃下静置沉淀过夜,再用卧式离心机以5000~7000r/min转速离心分离得到上清液;得到的上清液装入透析袋中,以1~2L流动的无水乙醇作为透析液,对上清液进行循环透析12~15h,收集循环透析后的无水乙醇放在旋转蒸发器中,在60~70℃下旋蒸浓缩至原体积的1/10,得到浓缩银杏果提取物,备用;称取400~500g人参茎叶放入气流粉碎机粉碎后按固液比为1:3将茎叶粉末和正丁醇混合,混合后倒入超声萃取仪中,在100~200W功率下超声萃取1~2h,过滤分离得到萃取液,将所得萃取液过大孔吸附树脂柱,再用大孔吸附树脂体积5~8倍的质量浓度75%无水乙醇对吸附树脂进行洗脱并收集洗脱液;将收集到的洗脱液放入蒸馏装置中,在60~70℃下蒸馏回收乙醇,得到人参皂甙,将100~200mL人参皂甙和200~300mL备用的浓缩银杏果提取物进行混合,得混合自由基清除剂粗品,放在棕色瓶中保存;量取100~200mL蓖麻油放入铁锅中,加热升温至100~110℃后,向油中加入10~20g壳聚糖,用铁勺不断搅拌,直至壳聚糖完全溶解,油糖混合液变粘稠后,使其自然冷却至室温,再加入等体积上述清除剂粗品混合均匀后,放入真空冻干机冻干后粉碎并过100目标准筛得粉末,包装后,即得一种包覆型自由基清除剂。
所述的大孔树脂为D101型大孔吸附树脂。
实例1
首先取1kg新鲜银杏果剥除果肉外层硬壳,将除壳后的银杏果和蒸馏水按体积比1:1进行混合后放入匀浆机中破碎匀浆,量取200mL破碎后的银杏果匀浆装入1L烧杯中,再向烧杯中加入匀浆体积2倍pH为7.6的磷酸盐缓冲液,用玻璃棒搅拌均匀;搅拌均匀后的混合液移入索式抽提器中抽提3h,量取300mL抽提液和100mL浓度0.5mol/L硫酸铵溶液放置在磁力搅拌机上搅拌均匀后移入冰水浴中,在4℃下静置沉淀过夜,再用卧式离心机以5000r/min转速离心分离得到上清液;得到的上清液装入透析袋中,以1L流动的无水乙醇作为透析液,对上清液进行循环透析12h,收集循环透析后的无水乙醇放在旋转蒸发器中,在60℃下旋蒸浓缩至原体积的1/10,得到浓缩银杏果提取物,备用;称取400g人参茎叶放入气流粉碎机粉碎后按固液比为1:3将茎叶粉末和正丁醇混合,混合后倒入超声萃取仪中,在100W功率下超声萃取1h,过滤分离得到萃取液,将所得萃取液过大孔吸附树脂柱,再用大孔吸附树脂体积5倍的质量浓度75%无水乙醇对吸附树脂进行洗脱并收集洗脱液;将收集到的洗脱液放入蒸馏装置中,在60℃下蒸馏回收乙醇,得到人参皂甙,将100mL人参皂甙和200mL备用的浓缩银杏果提取物进行混合,得混合自由基清除剂粗品,放在棕色瓶中保存;量取100mL蓖麻油放入铁锅中,加热升温至100℃后,向油中加入10g壳聚糖,用铁勺不断搅拌,直至壳聚糖完全溶解,油糖混合液变粘稠后,使其自然冷却至室温,再加入等体积上述清除剂粗品混合均匀后,放入真空冻干机冻干后粉碎并过100目标准筛得粉末,包装后,即得一种包覆型自由基清除剂。
所述的大孔树脂为D101型大孔吸附树脂。
本发明制备得到的自由基清除剂可以添加到保健品、化妆品和医药中,也可以作为食品添加保护剂,人体从膳食中补充自由基清除剂,从而达到防御疾病、延缓衰老的目的。
实例2
首先取1.5kg新鲜银杏果剥除果肉外层硬壳,将除壳后的银杏果和蒸馏水按体积比1:1进行混合后放入匀浆机中破碎匀浆,量取225mL破碎后的银杏果匀浆装入1L烧杯中,再向烧杯中加入匀浆体积2.5倍pH为7.6的磷酸盐缓冲液,用玻璃棒搅拌均匀;搅拌均匀后的混合液移入索式抽提器中抽提4h,量取350mL抽提液和125mL浓度0.5mol/L硫酸铵溶液放置在磁力搅拌机上搅拌均匀后移入冰水浴中,在5℃下静置沉淀过夜,再用卧式离心机以6000r/min转速离心分离得到上清液;得到的上清液装入透析袋中,以1.5L流动的无水乙醇作为透析液,对上清液进行循环透析14h,收集循环透析后的无水乙醇放在旋转蒸发器中,在65℃下旋蒸浓缩至原体积的1/10,得到浓缩银杏果提取物,备用;称取450g人参茎叶放入气流粉碎机粉碎后按固液比为1:3将茎叶粉末和正丁醇混合,混合后倒入超声萃取仪中,在150W功率下超声萃取1.5h,过滤分离得到萃取液,将所得萃取液过大孔吸附树脂柱,再用大孔吸附树脂体积6倍的质量浓度75%无水乙醇对吸附树脂进行洗脱并收集洗脱液;将收集到的洗脱液放入蒸馏装置中,在65℃下蒸馏回收乙醇,得到人参皂甙,将150mL人参皂甙和250mL备用的浓缩银杏果提取物进行混合,得混合自由基清除剂粗品,放在棕色瓶中保存;量取150mL蓖麻油放入铁锅中,加热升温至105℃后,向油中加入15g壳聚糖,用铁勺不断搅拌,直至壳聚糖完全溶解,油糖混合液变粘稠后,使其自然冷却至室温,再加入等体积上述清除剂粗品混合均匀后,放入真空冻干机冻干后粉碎并过100目标准筛得粉末,包装后,即得一种包覆型自由基清除剂。
所述的大孔树脂为D101型大孔吸附树脂。
本发明制备得到的自由基清除剂可以添加到保健品、化妆品和医药中,也可以作为食品添加保护剂,人体从膳食中补充自由基清除剂,从而达到防御疾病、延缓衰老的目的。
实例3
首先取2kg新鲜银杏果剥除果肉外层硬壳,将除壳后的银杏果和蒸馏水按体积比1:1进行混合后放入匀浆机中破碎匀浆,量取250mL破碎后的银杏果匀浆装入1L烧杯中,再向烧杯中加入匀浆体积3倍pH为7.6的磷酸盐缓冲液,用玻璃棒搅拌均匀;搅拌均匀后的混合液移入索式抽提器中抽提5h,量取400mL抽提液和150mL浓度0.5mol/L硫酸铵溶液放置在磁力搅拌机上搅拌均匀后移入冰水浴中,在6℃下静置沉淀过夜,再用卧式离心机以7000r/min转速离心分离得到上清液;得到的上清液装入透析袋中,以2L流动的无水乙醇作为透析液,对上清液进行循环透析15h,收集循环透析后的无水乙醇放在旋转蒸发器中,在70℃下旋蒸浓缩至原体积的1/10,得到浓缩银杏果提取物,备用;称取500g人参茎叶放入气流粉碎机粉碎后按固液比为1:3将茎叶粉末和正丁醇混合,混合后倒入超声萃取仪中,在200W功率下超声萃取2h,过滤分离得到萃取液,将所得萃取液过大孔吸附树脂柱,再用大孔吸附树脂体积8倍的质量浓度75%无水乙醇对吸附树脂进行洗脱并收集洗脱液;将收集到的洗脱液放入蒸馏装置中,在70℃下蒸馏回收乙醇,得到人参皂甙,将200mL人参皂甙和300mL备用的浓缩银杏果提取物进行混合,得混合自由基清除剂粗品,放在棕色瓶中保存;量取200mL蓖麻油放入铁锅中,加热升温至110℃后,向油中加入20g壳聚糖,用铁勺不断搅拌,直至壳聚糖完全溶解,油糖混合液变粘稠后,使其自然冷却至室温,再加入等体积上述清除剂粗品混合均匀后,放入真空冻干机冻干后粉碎并过100目标准筛得粉末,包装后,即得一种包覆型自由基清除剂。
所述的大孔树脂为D101型大孔吸附树脂。
本发明制备得到的自由基清除剂可以添加到保健品、化妆品和医药中,也可以作为食品添加保护剂,人体从膳食中补充自由基清除剂,从而达到防御疾病、延缓衰老的目的。
Claims (2)
1.一种包覆型自由基清除剂的制备方法,其特征在于具体制备步骤为:
(1)取1~2kg新鲜银杏果剥除果肉外层硬壳,将除壳后的银杏果和蒸馏水按体积比1:1进行混合后放入匀浆机中破碎匀浆,量取200~250mL破碎后的银杏果匀浆装入1L烧杯中,再向烧杯中加入匀浆体积2~3倍pH为7.6的磷酸盐缓冲液,用玻璃棒搅拌均匀;
(2)将上述搅拌均匀后的混合液移入索式抽提器中抽提3~5h,量取300~400mL抽提液和100~150mL浓度0.5mol/L硫酸铵溶液放置在磁力搅拌机上搅拌均匀后移入冰水浴中,在4~6℃下静置沉淀过夜,再用卧式离心机以5000~7000r/min转速离心分离得到上清液;
(3)将上述得到的上清液装入透析袋中,以1~2L流动的无水乙醇作为透析液,对上清液进行循环透析12~15h,收集循环透析后的无水乙醇放在旋转蒸发器中,在60~70℃下旋蒸浓缩至原体积的1/10,得到浓缩银杏果提取物,备用;
(4)称取400~500g人参茎叶放入气流粉碎机粉碎后按固液比为1:3将茎叶粉末和正丁醇混合,混合后倒入超声萃取仪中,在100~200W功率下超声萃取1~2h,过滤分离得到萃取液,将所得萃取液过大孔吸附树脂柱,再用大孔吸附树脂体积5~8倍的质量浓度75%无水乙醇对吸附树脂进行洗脱并收集洗脱液;
(5)将上述收集到的洗脱液放入蒸馏装置中,在60~70℃下蒸馏回收乙醇,得到人参皂甙,将100~200mL人参皂甙和200~300mL备用的浓缩银杏果提取物进行混合,得混合自由基清除剂粗品,放在棕色瓶中保存;
(6)量取100~200mL蓖麻油放入铁锅中,加热升温至100~110℃后,向油中加入10~20g壳聚糖,用铁勺不断搅拌,直至壳聚糖完全溶解,油糖混合液变粘稠后,使其自然冷却至室温,再加入等体积上述清除剂粗品混合均匀后,放入真空冻干机冻干后粉碎并过100目标准筛得粉末,包装后,即得一种包覆型自由基清除剂。
2.根据权利要求1所述的一种包覆型自由基清除剂的制备方法,其特征在于:所述的步骤(4)中大孔树脂为D101型大孔吸附树脂。
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CN107469066A (zh) * | 2017-08-23 | 2017-12-15 | 上海新肌生物科技有限公司 | 一种消除98%糖化反应链发生源的源头型抗糖化配方 |
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CN107281463A (zh) * | 2017-08-23 | 2017-10-24 | 上海新肌生物科技有限公司 | 一种可以清除99%的自由基产生源的综合型自由基清除方法 |
CN107469066A (zh) * | 2017-08-23 | 2017-12-15 | 上海新肌生物科技有限公司 | 一种消除98%糖化反应链发生源的源头型抗糖化配方 |
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