CN104560378A - 蓝莓籽油及其制备方法和应用 - Google Patents
蓝莓籽油及其制备方法和应用 Download PDFInfo
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- CN104560378A CN104560378A CN201310521687.9A CN201310521687A CN104560378A CN 104560378 A CN104560378 A CN 104560378A CN 201310521687 A CN201310521687 A CN 201310521687A CN 104560378 A CN104560378 A CN 104560378A
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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Abstract
本发明公开了一种蓝莓籽油及其制备方法和应用,所述蓝莓籽油采用下述一种或几种提取方法制得:有机溶剂浸提法;超临界萃取法;物理挤压法即得的蓝莓籽油,以上述蓝莓籽油为活性成分,辅以具有保健功能的物质和/或保健食品上可接受的辅料制成的剂型;上述蓝莓籽油和蓝莓籽油制剂在制备改善视力和降血脂保健食品上的应用。本发明采用物理挤压法、有机溶剂萃取和CO2超临界萃取法三种方法单独或者联合使用,确保了蓝莓籽油的出油率;该方法生产效率高,出油率高,成本低,技术可靠,经济易行;且适用范围广,大、中、小企业均可采用。
Description
技术领域
本发明涉及植物籽油的制备方法,特别涉及一种蓝莓籽油及其制备方法和应用。
背景技术
蓝莓是一种大众喜爱的水果,近年来越来越多的人认识到蓝莓的药用和营养价值。目前,我国蓝莓行业进入了一个新的发展时期,种植业和酒业、饮料的产业化加工发展已有一定的规模。然而在蓝莓鲜果中,蓝莓籽的含量约为3%,每年约产生几千吨蓝莓籽,而其大部分均被废弃掉;这不仅造成资源的巨大浪费,也会污染环境。然而到目前为止,在世界范围内对蓝莓籽的研究及对其的开发较少,因此,对蓝莓籽的研究及如何充分利用蓝莓籽即对蓝莓籽的综合利用,是目前亟待解决的问题。
发明内容
基于此,本发明的目的在于提供一种蓝莓籽油及其制备方法和应用。
解决上述技术问题的具体技术方案如下:
一种蓝莓籽油的制备方法,所述蓝莓籽油采用下述一种或几种提取方法制得:
(1)有机溶剂浸提法
将蓝莓籽用有机溶剂于50-80℃浸提或超声提取,回收有机溶剂,分液取油相,即可;
(2)超临界萃取法:萃取压力为29-34MPa,萃取温度为38-40℃,CO2流量为31-33Kg/h,分离压力为8-9MPa,分离温度为33-34℃,萃取时间为1.5-1.8h;
(3)物理挤压法:所述挤压的温度为45-55℃。
在其中一些实施例中,所述有机溶剂为石油醚或体积分数为60-80%的乙醇溶液。
在其中一些实施例中,蓝莓籽油的制备方法包括物理挤压法和有机溶剂浸提法,具体步骤如下:
(1)采用物理挤压法,得蓝莓籽油和蓝莓籽渣,将蓝莓籽油于0-60℃的低温恒温放置40min;
(2)将步骤(1)所述蓝莓籽渣用体积分数为60-80%的乙醇溶液于60-70℃提取2h,回收乙醇,去除水相,得提取液;
(3)合并步骤(1)所述蓝莓籽油和步骤(2)所述提取液,并用活性炭脱色,过滤,即得。
一种根据上述制备方法制得的蓝莓籽油。
在其中一些实施例中,所述蓝莓籽油占蓝莓籽的质量百分数为6-9%,所述蓝莓籽油中含有3-5wt%的视黄醛,91-93wt%的不饱和脂肪酸。
一种蓝莓籽油制剂,所述蓝莓籽油制剂:以上述的蓝莓籽油为活性成分,辅以具有保健功能的物质和/或保健食品上可接受的辅料制成的制剂。
在其中一些实施例中,所述制剂的剂型为片剂、口服液、软胶囊或硬胶囊。
一种蓝莓籽油和蓝莓籽油制剂在制备改善视力、降血脂、抗氧化、抗肿瘤、抗辐射、抗过敏、抗衰老、抗疲劳、增强记忆力保健食品上的应用。
本发明所述一种蓝莓籽油及其制备方法、应用和其制得的蓝莓籽制剂具有以下优点和有益效果:
(1)本发明所述蓝莓籽油的制备方法,采用物理挤压法、有机溶剂萃取和CO2超临界萃取法三种方法单独或者联合使用,降低了有机溶剂的残留量,确保了蓝莓籽油的出油率;该方法生产效率高,出油率高,成本低,技术可靠,经济易行;且适用范围广,大、中、小企业均可采用。
(2)本发明所述蓝莓籽油制备方法中采用的CO2超临界萃取法,所制得的蓝莓籽油具有显著的改善视力、缓解视疲劳和调节血脂的功效。
(3)本发明以蓝莓籽油为活性成分制成直接食用的蓝莓籽油制剂,变废为宝,避免了资源的浪费和环境的污染。
(4)本发明所述的蓝莓籽油制剂可根据不同的保健功能,以蓝莓籽油为主,辅以其他功能性成分,既可以保证蓝莓籽的功效,也可以增强蓝莓籽油的功能。
具体实施方式
为了能够更清楚地理解本发明的技术内容,特举以下实施例详细说明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。下列实施例中未注明具体条件的实验方法,测定方法,通常按照常规条件,或按照制造厂商所建议的条件。实施例中所用到的各种常用化学试剂,均为市售产品。
本发明所制得的蓝莓籽油中含有丰富的脂肪酸,含有较高的不饱和脂肪酸(91.20%以上),黄酮类、多糖类、花青素、芦丁、氨基酸、胡萝卜素、维生素A、视黄醛等多种活性成分,具有缓解视疲劳、美肤养颜、调节血脂、健身提神、抗氧化、抗肿瘤、抗辐射、抗过敏、抗衰老、抗疲劳、增强记忆力等功效,尤其缓解视疲劳、调节血脂等特别突出。
以下将结合具体实施例对本发明做进一步说明。
下述实施例中TPA是指12-氧-十四烷酰佛波醇-13-乙酸酯;
IC50又称半抑制浓度或称半抑制率,是指被抑制一半时抑制剂的浓度,这里的反应可以是酶催化反应,抗原抗体反应等。
实施例1
一种蓝莓籽油的制备方法,包括如下步骤:
(1)将蓝莓籽用清水洗净、烘干,于挤压机中压榨,得蓝莓籽油和蓝莓籽渣,将蓝莓籽油于0℃恒温放置40min待用;
(2)将上述蓝莓籽渣用体积分数为70%的乙醇溶液于65℃提取2h,回收乙醇,去除水相,取油相;
(3)合并上述蓝莓籽油和油相,并用活性炭脱色,过滤,即得。
本实施例所制得的蓝莓籽油占蓝莓籽的质量百分比为6.5%;经气相色谱分析,其纯度达96%。
实施例2
一种蓝莓籽油的制备方法,具体步骤与实施例1基本相同,区别在于:本实施例采用石油醚进行提取。本实施例所制得的蓝莓籽油占蓝莓籽的质量百分比为6%;经气相色谱分析,其纯度达96%。
实施例3
一种蓝莓籽油的制备方法,包括如下步骤:
(1)粉碎:将蓝莓籽粉碎至50-55目,每升反应釜中投加蓝莓籽粉末260g;
(2)萃取:萃取压力为32MPa,萃取温度为39℃,CO2流量为32Kg/h,
分离压力为8MPa,分离温度为33℃,萃取时间为1.6h;
本实施例所制得的蓝莓籽油占蓝莓籽的质量百分比为9%;经气相色谱分析,其纯度达98%。
实施例4蓝莓籽油的功效评价
一、蓝莓籽油的对视力的功效
(1)实验目的
通过实验,评价实施例1-3制得的蓝莓籽油的对视力的功效。
(2)实验方法
给予50例因长期在显示屏前工作的眼疲劳患者每天服用蓝莓籽油300mg,2个月后,考量其相对敏感性和客观症状;给予50名近视性视网膜非炎性改变的患者服用蓝莓籽油,每日150mg,2个月后,通过试验前后比较,考量受视者的视力。
(3)实验结果
结果表明:眼疲劳患者分别服用实施例1-3所制的蓝莓籽油2个月后,其中,服用实施例1、实施例2制得的蓝莓籽油的眼疲劳患者,其相对敏感性和客观症状有所改善;服用实施例3制得的蓝莓籽油的眼疲劳患者,其相对敏感性和客观症状有显著改善(P<0.05);近视性视网膜非炎性改变的患者分别服用实施例1-3所制的蓝莓籽油2个月后,其中,服用实施例1、实施例2制得的蓝莓籽油的患者视力有所提高,服用实施例3制得的蓝莓籽油的患者视力显著提高(P<0.05)。
经GC-MS测定:色谱条件:进样口温度280℃,分流进样,分流比29.1,压力100kPa,柱箱温度:初温80℃,保持2min,再以8℃/min的速率上升至200℃,保持2min,再以1℃/min的速率上升至210℃,保持2min,再以6℃/min的速率上升至280℃,保持10min,载气为氦气,恒线速44.5cm/s,流量为1.46ml/min。
经分析测定:蓝莓籽油中含有4%的视黄醛、β-胡萝卜素等增强视网膜的营养成分,可以改善视网膜功能和提高其灵敏度的作用。
二、蓝莓籽粉的降血脂功效
(1)实验目的
通过实验评价实施例1-3制得的蓝莓籽油降血脂的功效。
(2)实验方法
选择以高脂饲料(含猪油、胆固醇3%、猪胆盐0.5%和甲基硫氧嘧啶0.2%)喂食动物造成大鼠高血脂模型,以出血时间、凝血时间、血脂水平和抗自由基活性为药理指标,对蓝莓籽进行研究。在室温27℃,湿度60%的条件下,将动物饲养一周后,随机分为空白对照组、高血脂模型组、溶媒对照组(水溶液)、地奥心血康组(0.5mg甾体总皂苷/kg)、蓝莓籽提取物药组(50%醇提液)。除溶媒对照组8只外,其余各组每组10只动物。除空白对照组喂普通饲料外,其余各组均给予高脂饲料,连续饲养14天后,检查前一天禁食不禁饮8小时以上,每只动物均经眼球采血检测血脂,确认造模成功(给药前血脂水平,经过检验剔除血脂不升高的大鼠若干只)。随后继续给予高脂饮食。高脂饲料饲养约第15天开始给药,各实验药物组分别经灌胃口服给药,灌胃量为相当于生药3g·kg-1,每天一次,连续给药共四周28天,(末次给药后,禁食不禁饮8h)测大鼠出血时间、凝血时间。全部动物经眼眶采血,取血清,检测血脂(给药后血脂)和脂质过氧化物酶水平。
(3)实验结果
实施例1-3所制的蓝莓籽油受试药各组均在不同水平降低总胆固醇(TC)、甘油三酯(TG)。与高脂模型组和溶媒对照组比较,实施例1-2受试药组总胆固醇(TC)水平和甘油三酯(TG)略微降低,实施例3受试药组总胆固醇(TC)水平和甘油三酯(TG)显著降低(P<0.05)。对脂蛋白尤其是HDL/LDL比值的影响,从本实验结果来看,地奥心血康组对提升HDL水平,改善HDL/LDL比值效果一般,但是实施例1-2蓝莓籽油对于升高HDL水平效果略好,实施例3蓝莓籽油对于升高HDL水平效果较好,可以明显提高HDL/LDL比值,效果好于地奥心血康组(P<0.05)。
三、蓝莓籽油的抗脂质过氧化和清除自由基功效
(1)实验目的
通过比较实施例1制得的蓝莓籽油、VC、VE对TPA诱导的肝、脑组织中脂质过氧化的保护,评价蓝莓籽油的抗脂质过氧化和清除自由基功效。
(2)实验方法:分别使用化学发光法和细胞色素C还原法测定蓝莓籽油、VC、VE对活性氧即超氧阴离子自由基和羟基自由基的清除能力。
(3)实验结果
结果表明:在100mg/kg剂量下蓝莓籽油、VC、VE均可降低TPA诱导产生的活性氧,使用腹腔巨噬细胞发光法测定,活性氧的降低率分别为72%、19%、和45%,使用细胞色素还原法测定,活性氧的降低率分别为66%、16%和36%,同时还发现蓝莓籽油对于抑制TPA诱导的腹腔巨噬细胞活性氧的产生,具有剂量反应关系。因此,蓝莓籽油可对氧化损伤起到保护作用,且保护作用优于其它抗氧化剂。
具体来讲,蓝莓籽油对自由基的抑制具有浓度反应关系,在100mg/L的浓度时,蓝莓籽油对超氧化阴离子和羟基自由基的抑制能力为79%和82%:同等条件下,VC抑制上述两种自由基的能力为14%和21%,VE为49%和71%,说明蓝莓籽油是一种比VC、VE更强的自由基清除剂,其可应用于各种抗氧化、抗衰老产品中
四、蓝莓籽油的抗肿瘤功效
(1)实验目的
通过分析实施例1制得的蓝莓籽油对人肺癌细胞A549、人肝癌细胞HePG2、慢性骨髓性白血病细胞K562、正常人的胃粘膜细胞和正常鼠的巨噬细胞J774A.1的作用,评价蓝莓籽油的抗肿瘤功效。
(2)实验方法
采用MTT法,体外培养拮抗肿瘤研究法。
(3)实验结果
结果表明:蓝莓籽油对人肺癌细胞A549,人肝癌细胞HePG2有明显的抑制作用。而对慢性骨髓性白血病细胞K562无细胞毒作用,对正常人的胃粘膜细胞和正常鼠的巨噬细胞J774A.1却有促进增长,增强生长活力的作用。
五、蓝莓籽油的抗辐射功效
(1)实验目的
通过对比分析,评价实施例1制得的蓝莓籽油的抗辐射功效。
(2)实验方法
将荷Slao肉瘤小鼠分为对照组和实验组,实验组中分别给予4Co局部照射、口服蓝莓籽油和局部照射加口服蓝莓籽油的不同方法处理,持续12天后,检测动物的瘤重、白细胞计数、脾淋巴细胞转化率等指标。
(3)实验结果
结果表明:对照组瘤重高于其它各组,照射加口服高剂量蓝莓籽油的肿瘤抑制率高于单纯照射组和单纯口服蓝莓籽油组,单纯照射组的白细胞计数低于其它各组。表明蓝莓籽油可抑制辐照引发的脂质过氧化。这可能是蓝莓籽油抗辐射损伤的主要原因。
六、蓝莓籽油的抗过敏及抗炎功效
(1)实验目的
通过对比分析,评价实施例1制得的蓝莓籽油的抗过敏及抗炎功效。
(2)实验方法
采用耳廓肿胀法、足趾肿胀法等经典抗炎试验研究。
(3)实验结果
结果表明:由于蓝莓籽油的抗氧化活性,使其可抑制诸如组织胺、5-羟色胺、前列腺素及白三烯等炎症因子的合成和释放,抑制嗜碱细胞和肥大细胞释放过敏颗粒,从而有效地改善皮肤过敏症状及过敏性哮喘症状。
七、蓝莓籽油的抗衰老功效
(1)实验目的
通过分析,评价实施例1制得的蓝莓籽油的抗衰老功效。
(2)实验方法
通过体外抗酶实验,研究蓝莓籽油对黄嘌呤氧化酶、弹性蛋白酶、胶原蛋白酶、透明质酸酶、β-葡萄糖醛酸糖甙酶的IC50;并利用超临界萃取法,提取蓝莓籽油中视黄醛,以衡量蓝莓籽油的抗衰老功效。
(3)实验结果
蓝莓籽油的体外抗酶试验结果表明:蓝莓籽油对黄嘌呤氧化酶、弹性蛋白酶、胶原蛋白酶、透明质酸酶、β-葡萄糖醛酸糖甙酶的IC50(umol/1)分别为2.4、4,24、38、80、1.1;从中可以看出,蓝莓籽油对上述各酶具有显著的抑制作用。
而超临界萃取法提取蓝莓籽油中视黄醛结果表明:蓝莓籽油中含有4%的视黄醛,且其可以明显的改善皮肤的老化,减轻皮肤粗糙、皱纹、降低色斑沉积等功效。同时蓝莓籽油具有清除自由基,阻断弹性蛋白酶的产生并抑制其活性,从而改善皮肤健康状况。
八、蓝莓籽油的抗疲劳功效
(1)实验目的
通过分析,评价实施例1制得的蓝莓籽油的抗疲劳功效。
(2)实验方法
每天经口给予雄性昆明种小鼠高、中、低三种不同剂量的蓝莓籽油,剂量分别为:以体重计,低剂量1.7m/kg、中剂量16.7m/kg、高剂量50.0m/kg,30天后测定负重游泳时间、血红蛋白及运动后血乳酸和肝糖元含量。
(3)实验结果
结果表明:各剂量组小鼠负重游时间均比对照组延长,中、高剂量组具有极显著差异(P<0.01),血红蛋白含量均高于对照组;各剂量组小鼠运动后血乳酸含量均低于对照组,高剂量组与对照组相比具有极显著差异(P<0.01,肝糖元含量均高于对照组,中、高剂量组与对照组相比分别具有显著和极显著差异(P<0.05,P<0.01)。因此,蓝莓籽油具有抗疲劳的功效。
九、蓝莓籽油对记忆力的影响
(1)实验目的
通过实验,分析评价实施例1制得的蓝莓籽油对记忆力的影响。
(2)实验方法
通过对小鼠D-半乳糖6周,制备小鼠衰老模型,同时给药蓝莓籽油,分别采用跳台法、Y形迷宫法测试小鼠的学习记忆力,并测定小鼠血液和脑组织的过氧化脂质:正常小鼠给予给药蓝莓籽油,连续19天,采用Morris水迷宫法测试小鼠的学习记忆能力。
(3)实验结果
实验结果表明,蓝莓籽油在D-半乳糖所致衰老小鼠在跳台法的测试中,可延长潜伏期,减少5分钟内错误次数对小鼠Y型迷路的测试中,能减少错误反应次数,提示蓝莓籽油对由D-半乳糖所致小鼠学习记忆障碍有明显的改善作用。在Morris水迷宫测试中,蓝莓籽油对正常小鼠的学习记忆难以进一步提高,但能明显改善正常小鼠信息的保持和再现能力,作用机制可能与其能降低血液和脑组织的过氧化脂质有关。
实施例5蓝莓籽油制剂-软胶囊
配方:蓝莓籽油300g,维生素A50g,β-胡萝卜素50g,辅料600g,制得2000粒软胶囊,每粒0.5g。
工艺步骤为:原料→混合→压丸→洗丸、干燥+选丸→内包装+外包装→成品。
本实施例所制得的软胶囊,以蓝莓籽油为主要成分,辅以功能性物质维生素A、β-胡萝卜素,其可用于缓解视疲劳。
实施例6蓝莓籽油制剂-硬胶囊
配方:蓝莓籽油50g,维生素E10g,维生素C20g,环状糊精等辅料220g,制成1000粒,每粒0.3g。
工艺步骤为:混料(80目)→制软材→制粒→装硬胶囊→压PVC→成品。
本实施例所制得的硬胶囊,以蓝莓籽油为主要成分,辅以功能性物质维生素E、维生素C,其可用于抗氧化。
实施例7蓝莓籽油制剂-片剂
配方:蓝莓籽油50g,维生素E10g,牛磺酸5g,环状糊精等辅料235g,制成1000粒,每粒0.3g。
工艺步骤为:混料→制软材→制粒→压片→包衣→压PVC板→成品。
本实施例所制得的片剂,以蓝莓籽油为主要成分,辅以功能性物质维生素E、牛磺酸C,其可用于抗疲劳。
实施例8蓝莓籽油制剂-口服液
配方:蓝莓籽油2000克,去离子水7920克,苯甲酸钠30克,硬脂酸单甘酯50克,香精适量,制成1000瓶,每瓶10ml。
工艺步骤为:混料→乳化→高压均质→罐封→灯检→包装→成晶。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (7)
1.一种蓝莓籽油的制备方法,其特征在于,所述蓝莓籽油采用下述一种或几种方法制得:
(1)有机溶剂浸提法
将蓝莓籽用有机溶剂于50-80℃浸提或超声提取,回收有机溶剂,分液取油相,即可;
(2)物理挤压法:所述挤压的温度为45-55℃;
(3)超临界CO2萃取法
所述超临界CO2萃取法中:萃取压力为29-34MPa,萃取温度为38-40℃,CO2流量为31-33Kg/h,分离压力为8-9MPa,分离温度为33-34℃,萃取时间为1.5-1.8h。
2.根据权利要求1所述的蓝莓籽油的制备方法,其特征在于,所述有机溶剂为石油醚或体积分数为60-80%的乙醇溶液。
3.根据权利要求1所述的蓝莓籽油的制备方法,其特征在于,包括物理压榨和有机溶剂浸提,具体步骤为:
(1)于45-55℃采用物理挤压法,得蓝莓籽油和蓝莓籽渣,将蓝莓籽油于0-60℃低温恒温放置40min;
(2)将步骤(1)所述蓝莓籽渣用石油醚或体积分数为60-80%的乙醇溶液于60-70℃提取2h,回收石油醚或乙醇,取油相;
(3)合并步骤(1)所述蓝莓籽油和步骤(2)所述油相,活性炭脱色,过滤,即可。
4.根据上述权利要求1-3任一项所述的制备方法制得的蓝莓籽油。
5.一种蓝莓籽油制剂,其特征在于,所述蓝莓籽油制剂以权利要求4所述蓝莓籽油为活性成分,辅以具有保健功能的物质和/或保健食品上可接受的辅料制成的制剂。
6.根据权利要求5所述的蓝莓籽油制剂,其特征在于,所述制剂的剂型为片剂、口服液、软胶囊、散剂、冲剂或硬胶囊。
7.一种如权利要求4所述的蓝莓籽油和权利要求5所述的蓝莓籽油制剂在制备改善视力、缓解视疲劳和降血脂的保健食品上的应用。
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