CN113413342B - 一种从澳洲坚果中提取棕榈油酸的方法及其应用 - Google Patents
一种从澳洲坚果中提取棕榈油酸的方法及其应用 Download PDFInfo
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- CN113413342B CN113413342B CN202110710928.9A CN202110710928A CN113413342B CN 113413342 B CN113413342 B CN 113413342B CN 202110710928 A CN202110710928 A CN 202110710928A CN 113413342 B CN113413342 B CN 113413342B
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- palmitoleic acid
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- mixed oil
- antioxidant
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- 235000021319 Palmitoleic acid Nutrition 0.000 title claims abstract description 60
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 title claims abstract description 60
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- 239000000284 extract Substances 0.000 claims abstract description 31
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Classifications
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Abstract
本发明涉及坚果果油制备技术领域,具体涉及一种从澳洲坚果中提取棕榈油酸的方法及其应用。一种从澳洲坚果中提取棕榈油酸的方法,使用减压蒸馏的方法纯化澳洲坚果的果油,在减压蒸馏过程中加入了抗氧化剂。该抗氧化剂由如下方法制备:使用乙醇热回流提取粉碎后的澳洲坚果青皮;先使用石油醚萃取青皮提取液,再使用乙酸乙酯萃取青皮提取液,取乙酸乙酯层,获得本方案的抗氧化剂。本方案可以解决提取和富集棕榈油酸的过程中油脂容易被氧化变质的技术问题,并可以将澳洲坚果的果油中的棕榈油酸富集3倍以上。本方案可以应用于棕榈油酸的制备和纯化的实践操作中,提升棕榈油酸的品质和扩大其应用领域。
Description
技术领域
本发明涉及坚果果油制备技术领域,具体涉及一种从澳洲坚果中提取棕榈油酸的方法及其应用。
背景技术
澳洲坚果(Macadamia integrifolia)是一种含油量高、营养丰富、香脆可口的食用坚果,食用部分为果仁,可生吃,烤制后酥脆,口感细腻,带有奶油清香,风味极佳。脂肪含量高达78%以上,而炒花生仁含脂肪仅44.8%,腰果仁47%,杏仁51%,核桃亦只有63%。澳洲坚果含多种脂肪酸,其中不饱和脂肪酸占总脂肪酸的84%。不饱和脂肪酸的生理功能包括:保持细胞膜的相对流动性,以保证细胞的正常生理功能;使胆固醇酯化,降低血中的胆固醇和甘油三酯;是合成人体内前列腺素和凝血恶烷的前躯物质;降低血液粘稠度,改善血液微循环;提高脑细胞的活性,增强记忆力和思维能力。
棕榈油酸是一种由16个碳原子组成且含有一个双键的ω-7单不饱和脂肪酸,在营养、医药和工业上具有重要的应用价值。棕榈油酸在自然界中的来源有限,主要为动物来源(例如,鲸鱼和鱼肝油),而植物中棕榈油酸的含量有限,但是,澳洲坚果果仁中含有比较大量的棕榈油酸。但是,现有技术中尚未见关于澳洲坚果棕榈油酸提取和富集的研究和报道。目前,澳洲坚果的果油的制备过程较为复杂和冗长,棕榈油酸在漫长的制备过程中容易被氧化变质,从而影响其生物学效应和产品品质,亟需开发一种能够提升棕榈油酸产品品质的从澳洲坚果的果仁中提取和富集棕榈油酸的方法。
发明内容
本发明意在提供一种从澳洲坚果中提取棕榈油酸的方法,以解决提取和富集棕榈油酸的过程中油脂容易被氧化变质的技术问题。
为达到上述目的,本发明采用如下技术方案:
一种从澳洲坚果中提取棕榈油酸的方法,包括以下依次进行的步骤:
S1:将从澳洲坚果的果仁中冷榨提取获得的果油依次进行皂化和酸化处理,获得混合油D;
S2:在混合油D中加入抗氧化剂,再对混合油D进行减压蒸馏处理,收集馏分,洗涤所述馏分并除去所述馏分中的水分后获得混合油G;
所述抗氧化剂由如下方法制备:
S1’:使用乙醇作为提取溶剂,热回流提取粉碎后的澳洲坚果青皮,获得醇提液;将醇提液浓缩为浸膏,将浸膏溶于水,获得水溶液A;
S2’:使用石油醚萃取水溶液A,取水层获得水溶液B;
S3’:使用乙酸乙酯萃取水溶液B,取乙酸乙酯层并浓缩后,获得所述抗氧化剂。
本方案的原理及优点是:通过皂化使得果油中的脂肪分解为脂肪酸盐,然后通过酸化将脂肪酸盐转化成脂肪酸。通过减压蒸馏的方式收集含有大量棕榈油酸的馏分,从而将棕榈油酸提取和富集。在减压蒸留的过程中,脂肪酸等容易被氧化,其功效会由于较长的制备过程而降低。所以在加圧蒸留过程中,最好能够加入一些抗氧化剂来防止棕榈油酸被氧化。现有技术中的抗氧化剂虽然能够起到一定程度上的抗氧化作用。在本方案中使用澳洲坚果青皮提取物来实现防止棕榈油酸被氧化的作用。发明人经过对青皮的大量研究发现,对青皮的醇提物使用石油醚萃取,保留水相,在对保留的水相进行乙酸乙酯萃取,取乙酸乙酯相,此部分的提取物具有较好的抗棕榈油酸氧化的作用,而使用其他的提取部分(例如石油醚提取部分,正丁醇提取部分等)却不具备上述作用。发明人发现了青皮的乙酸乙酯萃取部分在脂肪酸抗氧化上具有良好的作用,进而利用这个研究发现来制备和提取棕榈油酸,对提升棕榈油酸的质量起到了促进作用。澳洲坚果的青皮是澳洲坚果加工过程中被弃用的部分,而通过本方案可以将青皮进一步地利用,这是除了将青皮作为肥料之外的一大用途,为澳洲坚果青皮资源的综合利用提供了一条可行的途径。
进一步,在S1’中,使用体积分数为95%的乙醇作为提取溶剂,热回流提取粉碎后的澳洲坚果青皮3h,乙醇和澳洲坚果青皮的料液比为500mL:500g。采用上述提取溶剂、料液比和提取方式,可以将青皮中的具有抗氧化作用的成分充分提取。
进一步,在S2’中,使用石油醚萃取水溶液A三次;每次萃取时,石油醚和水溶液A的体积比为1:1。使用石油醚萃取水溶液A三次,可将溶液A中的非极性较强的部分分离进入石油醚相,而具有抗氧化作用的部分继续保留在水相中。
进一步,在S3’中,使用乙酸乙酯萃取水溶液B三次;每次萃取时,乙酸乙酯和水溶液B的体积比为1:1。使用乙酸乙酯萃取可将水溶液B中非极性相对较强的部分提取,极性较强的部分继续保留在水相中。经过试验研究证明,乙酸乙酯相中萃取出的成分具有较好的抗脂肪酸氧化的性能。
进一步,在S1中,将果油和氢氧化钠溶液充分混合均匀之后50℃反应4h,分层后获得水层和混合油A;使用盐酸溶液将所述水层的pH值调节为5,然后取混合油A,经水洗和干燥后,获得混合油D。采用上述技术方案,50℃皂化反应4h,果油中的脂肪被充分水解,形成脂肪酸盐和甘油,再通过酸化处理,脂肪酸盐形成脂肪酸,经水洗后,将脂肪酸的混合油中的碱充分清洗,以备进行后续的减压蒸馏过程。
进一步,在S2中,抗氧化剂在混合油D中的质量分数为1-4%。上述抗氧化剂的用量可以保证棕榈油酸在制备过程中不会被大量氧化分解。
进一步,在S2中,减压蒸馏处理的参数条件为80℃、-60MPa和4h。上述参数条件可以保证将棕榈油酸充分蒸馏,在获得的馏分中可以收集富集有棕榈油酸的产品。通过上述减压蒸馏的方法,可以将产品中的棕榈油酸的含量提高3倍以上。
进一步,所述混合油G用于制备药品、化妆品或者保健品。
棕榈油酸是由十六个碳原子组成且含有一个双键的单不饱和脂肪酸,是自然界中常见的omega-7脂肪酸之一。由于棕榈油酸在一些慢性疾病如代谢综合征、糖尿病和炎症中起到一定的治疗作用,已引起人们的广泛关注。棕榈油酸渗透皮肤速度快,使皮肤平滑、不油腻,目前棕榈油酸已开始应用于面部护肤、唇膏和婴儿制品以及防晒制品中。也有研究表明,棕榈油酸对小鼠黑色素瘤细胞的黑色素生成有较强的抑制作用,其在蛋白水平上抑制了小鼠黑色素细胞中酪氨酸酶的活性,从而减少了黑色素的合成。因此,棕榈油酸是一种有效的增白剂,可用于美白护肤品的制备中。采用本方案的方法,可以减少棕榈油酸在制备过程中的氧化变质,及大地提升棕榈油酸制品的品质。
进一步,所述混合油G的过氧化值小于7meq/kg。在本方案中,由于使用了来源于澳洲坚果青皮提取物的抗氧化剂,脂肪酸在提取和制备过程中,发生氧化分解的量减小,最大程度地保证了棕榈油酸的品质。
进一步,所述混合油G中棕榈油酸的质量分数大于50%。通过本方案可以将棕榈油酸富集,使得其质量分数提升至50%以上,以满足后续制备药品、化妆品和保健品的需求。
具体实施方式
下面通过具体实施方式进一步详细说明:
实施例1
对澳洲坚果的果仁采用常规冷榨工艺进行油脂压榨,获得果油。经检测,果油中含有52.12%的油酸,17.33%的棕榈油酸。本实施例对果油中的棕榈油酸进行提取和富集处理。在反应釜中,加入果油和溶质的质量分数为1%的氢氧化钠溶液,果油和氢氧化钠溶液的质量比为1:4。在本实施例中具体加入了1kg的果油进行提取和反应。将果油和氢氧化钠溶液充分混合均匀之后,50℃反应4h,反应釜中的物料出现水油分层(下层为水层和上层为混合油A),完成皂化反应。然后在物料中加入5mol/L的盐酸溶液,调节水层的pH值为5,然后取混合油A。在混合油A中按照体积比3:1的比例加入纯水,充分混合后静置分层,取上层的油相,获得混合油B。重复上述水洗操作,获得混合油C。在混合油C中加入无水硫酸钠,无水硫酸钠在混合油C中的质量分数为4%,搅拌30min,除去混合油C中的水分,过滤后获得混合油D(其中主要有各类脂肪酸),混合油D的重量为0.75kg。然后在混合油D中加入抗氧化剂,抗氧化剂在混合油D中的质量分数为3%。对含有抗氧化剂的混合油D中加入到减压蒸馏设备中,在80℃和-60MPa的条件下减压蒸馏4h,收集馏分。在馏分中加入按照5:1的比例加入纯水,充分混合后静置分层,取上层的油相,获得混合油E。重复上述水洗操作,获得混合油F。在混合油F中加入无水硫酸钠,无水硫酸钠在混合油F中的质量分数为4%,搅拌30min,除去混合油F中的水分,过滤后获得混合油G(其中主要有各类脂肪酸,以棕榈油酸为主),混合油G的重量为0.31kg,经检测,混合油G中的棕榈油酸的质量分数为53.61%,将棕榈油酸的含量提高了3倍。
本方案的抗氧化剂由如下方法制备:
称取澳洲坚果青皮干样500g(水分含量15%),将其粉碎加入500mL体积分数为95%的乙醇,热回流提取3h,然后过滤、抽滤,收集滤液。再加体积分数为95%的乙醇回流,共对药材回流处理3次,将三次获得的滤液合并,获得醇提液。然后将得到的青皮醇液烘干至膏状,获得浸膏(密度为1.31g/ml),将浸膏溶于纯水,每10g溶于500ml纯水,获得水溶液A备用。
使用等体积的石油醚萃取水溶液A,摇匀,静置萃取5小时,保留石油醚层。萃取过程重复三次,将石油醚层合并,获得石油醚提取液,同时保留经过石油醚萃取过后的水层,获得水溶液B。将石油醚提取液蒸干至膏状,获得浸膏(密度为1.20g/ml),即获得第一提取物。
使用等体积的乙酸乙酯萃取水溶液B,摇匀,静置萃取5小时,保留乙酸乙酯层,萃取过程重复三次,将乙酸乙酯层合并,获得乙酸乙酯提取液,同时保留经过乙酸乙酯萃取过后的水层,获得水溶液C。将乙酸乙酯提取液蒸干至膏状,获得浸膏(密度为1.35g/ml),即获得第二提取物。
使用等体积的正丁醇萃取水溶液C,摇匀,静置萃取5小时,保留正丁醇层,萃取过程重复三次,将正丁醇层合并,获得正丁醇提取液,同时保留经过正丁醇萃取过后的水层,获得水溶液D。将正丁醇提取液蒸干至膏状,获得浸膏(密度为1.33g/ml),即获得第三提取物。将水溶液D蒸干至膏状,获得浸膏(密度为1.25g/ml),即获得第四提取物。
在本实施例中,使用的抗氧化剂为第二提取物。抗氧化剂在混合油D中的质量分数为3%。按照《GB/T 5009.37-2005食用油卫生标准分析方法过氧化值测定》,对最终获得的混合油G的过氧化值进行检测,检测结果为5.369meq/kg。过氧化值表示油脂和脂肪酸等被氧化程度的一种指标,用于说明油脂样品是否已氧化变质,油脂氧化后生成过氧化物、醛、酮等。过氧化值是衡量油脂酸败程度,一般来说过氧化值越高其酸败就越高,油脂以及脂肪酸氧化酸败产生的一些小分子物质在体内对人体产生不良的影响,如产生自由基,所以过氧化值太高的油对会对身体健康产生负面影响。
实施例2:基本同实施例1,但是将抗氧化剂在混合油D中的质量分数调整为1%,混合油G的过氧化值检测结果为6.320meq/kg,混合油G中的棕榈油酸的质量分数为51.21%。
实施例3:基本同实施例1,但是将抗氧化剂在混合油D中的质量分数调整为4%,混合油G的过氧化值检测结果为5.014meq/kg,混合油G中的棕榈油酸的质量分数为52.36%。
对比例1:基本同实施例1,但是将抗氧化剂替换为第一提取物,混合油G的过氧化值检测结果为10.544meq/kg。
对比例2:基本同实施例1,但是将抗氧化剂替换为第三提取物,混合油G的过氧化值检测结果为12.752meq/kg。
对比例3:基本同实施例1,但是将抗氧化剂替换为第四提取物,混合油G的过氧化值检测结果为11.710meq/kg。
对比例4:基本同实施例1,但是不使用抗氧化剂,混合油G的过氧化值检测结果为18.322meq/kg。
对比例5:基本同实施例1,但是将抗氧化剂替换为迷迭香提取物(迷迭香酸含量80%),混合油G的过氧化值检测结果为5.018meq/kg。
综上所述,本方案(实施例1-3)在提取果油的棕榈油酸的过程中,使用了新型的抗氧化剂(澳洲坚果青皮的第二提取物),在减压蒸馏的过程中可以较好地保护果油中的脂肪酸成分不被氧化酸败,保证了提取获得的棕榈油酸的品质。第二提取物来源于青皮提取物的乙酸乙酯萃取部分,而青皮提取物的石油醚萃取部分、正丁醇萃取部分等在对于棕榈油酸的减压蒸馏过程的抗氧化效果,均不如乙酸乙酯萃取部分。采用本方案,可以将澳洲坚果的果油中的棕榈油酸富集3倍以上,且操作过程简单,整个过程中没有使用复杂且价格高昂的仪器。制作出的棕榈油酸品质较好,可以将制备出来的含棕榈油酸的混合油用于食品、保健品或者化妆品的制备和应用中,发挥棕榈油酸的美白、抗高血压和降血糖等功效。
采用现有技术中常用的迷迭香提取物,同样能达到较好的抗氧化效果。但是迷迭香提取物需要额外购买,增加了制作成本。而澳洲坚果的青皮是澳洲坚果加工过程中被弃用的部分,而通过本方案可以将青皮进一步地利用,这是除了将青皮作为肥料之外的一大用途,为澳洲坚果青皮资源的综合利用提供了一条可行的途径。
以上所述的仅是本发明的实施例,方案中公知的具体技术方案和/或特性等常识在此未作过多描述。应当指出,对于本领域的技术人员来说,在不脱离本发明技术方案的前提下,还可以作出若干变形和改进,这些也应该视为本发明的保护范围,这些都不会影响本发明实施的效果和专利的实用性。本申请要求的保护范围应当以其权利要求的内容为准,说明书中的具体实施方式等记载可以用于解释权利要求的内容。
Claims (7)
1.一种从澳洲坚果中提取棕榈油酸的方法,其特征在于,包括以下依次进行的步骤:
S1:将从澳洲坚果的果仁中冷榨提取获得的果油依次进行皂化和酸化处理,获得混合油D;
S2:在混合油D中加入抗氧化剂,再对混合油D进行减压蒸馏处理,收集馏分,洗涤所述馏分并除去所述馏分中的水分后获得混合油G;
所述抗氧化剂由如下方法制备:
S1’:使用乙醇作为提取溶剂,热回流提取粉碎后的澳洲坚果青皮,获得醇提液;将醇提液浓缩为浸膏,将浸膏溶于水,获得水溶液A;
S2’:使用石油醚萃取水溶液A,取水层获得水溶液B;
S3’:使用乙酸乙酯萃取水溶液B,取乙酸乙酯层并浓缩后,获得所述抗氧化剂;
在S1’中,使用体积分数为95%的乙醇作为提取溶剂,热回流提取粉碎后的澳洲坚果青皮3h,乙醇和澳洲坚果青皮的料液比为500mL:500g;
在S2’中,使用石油醚萃取水溶液A三次;每次萃取时,石油醚和水溶液A的体积比为1:1;
在S3’中,使用乙酸乙酯萃取水溶液B三次;每次萃取时,乙酸乙酯和水溶液B的体积比为1:1。
2.根据权利要求1所述的一种从澳洲坚果中提取棕榈油酸的方法,其特征在于,在S1中,将果油和氢氧化钠溶液充分混合均匀之后50℃反应4h,分层后获得水层和混合油A;使用盐酸溶液将所述水层的pH值调节为5,然后取混合油A,经水洗和干燥后,获得混合油D。
3.根据权利要求2所述的一种从澳洲坚果中提取棕榈油酸的方法,其特征在于,在S2中,抗氧化剂在混合油D中的质量分数为1-4%。
4.根据权利要求3所述的一种从澳洲坚果中提取棕榈油酸的方法,其特征在于,在S2中,减压蒸馏处理的参数条件为80℃、-60MPa和4h。
5.根据权利要求1-4任一项所述的一种从澳洲坚果中提取棕榈油酸的方法的应用,其特征在于,所述混合油G用于制备药品、化妆品或者保健品。
6.根据权利要求5所述的一种从澳洲坚果中提取棕榈油酸的方法的应用,其特征在于,所述混合油G的过氧化值小于7meq/kg。
7.根据权利要求6所述的一种从澳洲坚果中提取棕榈油酸的方法的应用,其特征在于,所述混合油G中棕榈油酸的质量分数大于50%。
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