CN109984975A - 一种薄壳山核桃饼粕中具有抗氧化活性总酚的制备方法及用途 - Google Patents
一种薄壳山核桃饼粕中具有抗氧化活性总酚的制备方法及用途 Download PDFInfo
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract
本发明涉及一种从薄壳山核桃榨油副产物饼粕中提取得到具有抗氧化活性总酚的制备方法及用途。其特征在于制备方法包括采用薄壳山核桃榨油副产物饼粕为原料,乙醇回流提取后,大孔树脂柱层析,采用20‑40%的乙醇洗脱得到酚类物质集中的活性部位。本发明的提取工艺及方法适用于工业化生产,获得的薄壳山核桃总酚得率及纯度高,主要活性成分儿茶素、鞣花酸和EGCG之和不少于15%。薄壳山核桃总酚具有显著的抗氧化活性,可用于制备具有抗氧化功效的保健品或化妆品。
Description
技术领域
本发明属于农业领域,具体涉及一种薄壳山核桃饼粕中具有抗氧化活性总酚的制备方法及用途。
背景技术
薄壳山核桃[Carya illinoensis(Wangech.)K.Koch]为胡桃科(Juglandaceae)山核桃属(Carya)多年生高大乔木,又名美国山核桃、长山核桃,其果实富含油脂,可榨油。薄壳山核桃油中不饱和脂肪酸比例高,饱和脂肪酸比例低,不含反式脂肪酸,还含有丰富的维生素E、角鲨烯、磷脂等,对心脑血管具有良好的保健作用。我国目前食用油原料有很大比例依赖进口,且与发达国家相比木本食用油比例明显偏低。薄壳山核桃含油率高,且所榨的油对人体有诸多健康功效,有望成为继橄榄油后的又一高档木本油品。近年来,国家大力支持木本油料产业发展,我国多个省份,如江苏、安徽、浙江、江西等,均大力发展薄壳山核桃产业,种植面积快速上升。国产薄壳山核桃果实及薄壳山核桃油均大量上市销售,而榨油后的副产物—饼粕如何利用目前研究较少。
除油脂外,薄壳山核桃果实中还含有另一类重要的营养物质—酚类。2004年,美国的Ronald L.Prior研究团队测定了美国市场上售卖的100种常见食品,发现薄壳山核桃种仁在干果中抗氧化性排名第一,显著高于其他干果,且高于许多已知的富含酚类的水果和蔬菜,这一研究结果引起了人们对薄壳山核桃中抗氧化性物质的广泛关注。同年,美国的另一个研究团队调查了98种常见食品中的酚类物质含量,结果显示薄壳山核桃种仁含量排名第二,仅次于烘烤过的黑巧克力,且高于人们熟知的抗氧化活性强的蓝莓、黑莓等浆果。之后,美国农业部总结为:“薄壳山核桃是抗氧化剂含量最高的坚果”,并在广大民众中广泛推广这一概念,来推动人们每日食用具有健康益处的薄壳山核桃果仁。
薄壳山核桃果实中的酚类物质极性较大,主要存在于薄壳山核桃的非油部分,具有显著的抗氧化活性。薄壳山核桃中的酚类物质主要包含单宁、黄酮和单体酚酸,其中最主要的结构类型是鞣花酸及其衍生物,如鞣花酸糖苷、甲基鞣花酸及其糖苷,其次是儿茶素及其衍生物,如儿茶素糖苷、由儿茶素聚合而成的原花青素等,另外,薄壳山核桃成熟种仁中含量较高的酚类物质还有表没食子酸儿茶素没食子酸酯(Epigallocatechin gallate,EGCG)。已有试验证明活性氧过量累积会导致炎症,许多慢性疾病的发生与炎症密切相关。食用薄壳山核桃可降低血液的过氧化程度,从而抑制或延缓许多慢性疾病的发生。如Domínguez-Avila等通过小鼠体内试验证明薄壳山核桃总酚可降低血液脂质的过氧化程度、上调载脂蛋白B和LDL受体mRNA在肝脏中的表达,即发挥降血脂和抗氧化的功效。Robbins等的小鼠体内试验结果表明,薄壳山核桃中的酚类物质粗提物可抑制小鼠RAW 264.7巨噬细胞释放NO和过氧化,即具有抗炎作用。薄壳山核桃中富含的抗氧化酚类物质也有利于缓解其他一些疾病,如过量摄入烟草、酒精带来的过氧化症状,保护大脑、血液和肝部健康。
薄壳山核桃榨油后的副产物—饼粕仍含有大量具有抗氧化活性的酚类物质。目前榨油后的饼粕主要用来饲用或沤制饼肥,附加值较低,造成资源浪费。通过简单分离纯化,获取薄壳山核桃总酚,可应用于食品、保健品、化妆品行业添加。本专利工艺采用乙醇提取,大孔树脂纯化,全程不涉及有机溶剂及酸碱试剂,工艺简单、成本低廉、环境友好、产品无残留,适用于工业化生产。
发明内容
针对本领域的不足之处,本发明的目的是提供一种从薄壳山核桃榨油后的饼粕中提取具有抗氧化活性的总多酚的制备工艺及用途,该方法可用于工业化生产。
为实现上述目的,本发明采用的技术方案为:
一种薄壳山核桃饼粕中具有抗氧化活性酚类物质的制备方法,其特征在于,包括以下步骤:
(1)取薄壳山核桃榨油后的饼粕,加入一定比例的乙醇回流提取1-3次,合并提取液,回收溶剂至无醇味;
(2)提取液采用大孔树脂纯化,提取液吸附流速为1BV/h,上样后先用2-3BV的水洗除杂,水洗脱流速为2-3BV/h,再用乙醇洗脱,乙醇用量为2-4BV,乙醇洗脱流速为1-2BV/h;
(3)收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚。
步骤(1)中乙醇浓度为50-90%,料液比为1:10-18,提取温度为60-90℃,提取时间为1-3h,提取3次。
步骤(2)中所用的大孔树脂型号为D101或AB-8,洗脱乙醇浓度为20-40%。
步骤(3)中所获得的薄壳山核桃总多酚,其总酚含量为200-400mg EAE·g-1,鞣花酸含量为5-8%,儿茶素含量为10-15%,EGCG含量为2-5%。
所述方法获得的薄壳山核桃总多酚在制备具有抗氧化功效的保健品和化妆品中的用途。
本发明的有益效果在于:
本发明提出了一种从薄壳山核桃榨油后剩余的饼粕残渣中提取具有显著抗氧化活性总酚的制备方法及用途,为薄壳山核桃的综合利用提供了方法,提高了薄壳山核桃的产品附加值。本发明工艺主要采用乙醇及大孔树脂,环保无毒、价格低廉、安全性高且可重复使用,适用于工业化生产。本发明根据薄壳山核桃中酚类物质的组成及结构特点,通过对不同流分的总酚含量进行监控测定,准确的找到了富含总酚的有效部位,使产物杂质更少,总酚含量更高,抗氧化性更好。本发明获得的总酚产物分别采用总酚含量和单体酚酸含量进行表征,使产品质量易于把控。
附图说明
图1不同乙醇浓度的影响试验图
图2不同料液比的影响试验图
图3不同提取温度的影响试验图
图4不同提取时间的影响试验图
图5不同溶剂对大孔树脂富集物总酚含量和抗氧化性的影响图
具体实施方式
以下将结合具体实施例对本发明做进一步的详细说明,但不用来限制本发明的范围。
BV为柱体积。
实施例1提取工艺优化
单因素试验分别考察乙醇浓度、料液比、提取温度和提取时间四个因素对提取率的影响。
乙醇浓度的影响试验取薄壳山核桃榨油后的饼粕,按照料液比1:10分别加入50%、60%、70%、80%、90%的乙醇,90℃回流提取1.5h,提取3次,合并提取液,回收溶剂至无醇味,真空干燥得粗提物,根据公式:提取率(%)=粗提物干样质量(g)/饼粕干样质量(g)×100%计算提取率,结果见图1。从图1可看出,提取率随乙醇浓度的升高而升高,乙醇浓度为70%时提取率达到最大值,之后略有下降,因此选择乙醇浓度60%、70%和80%三个水平进行正交试验。
料液比的影响试验取薄壳山核桃榨油后的饼粕,分别按照料液比1:10、1:12、1:14、1:16、1:18加入70%的乙醇,90度回流提取1.5h,提取3次,合并提取液,回收溶剂至无醇味,真空干燥得粗提物。计算提取率,结果见图2。从图2可看出,提取率随料液比的升高而升高,但综合考虑经济因素选择料液比1:10、1:12和1:14三个水平进行正交试验。
提取温度的影响试验取薄壳山核桃榨油后的饼粕,按照料液比1:10加入90%的乙醇,分别于60℃、70℃、80℃、90度回流提取1.5h,提取3次,合并提取液,回收溶剂至无醇味,真空干燥得粗提物。计算提取率,结果见图3。从图3可看出,提取率随提取温度升高而升高,提取温度为80℃时提取率达到最大值,之后略有下降,因此选择提取温度70℃、80℃、90℃三个水平进行正交试验。
提取时间的影响试验取薄壳山核桃榨油后的饼粕,按照料液比1:10加入70%的乙醇,分别于90℃回流提取1h、1.5h、2h、2.5h、3h,提取3次,合并提取液,回收溶剂至无醇味,真空干燥得粗提物。计算提取率,结果见图4。从图4可看出,提取率随提取时间的增加而升高,提取时间为1.5h时提取率升高趋势较明显,之后趋于平缓,综合考虑经济因素选择提取时间1h、1.5h和2h三个水平进行正交试验。
正交试验根据单因素得到的试验结果,以乙醇浓度、料液比、提取温度、提取时间4个试验因素,每个因素均为3水平,因素水平见表1,根据正交试验表L9(34)进行试验,结果见表2。从表2中可看出,最佳提取工艺为乙醇浓度70%、料液比1:14、提取温度70℃、提取时间2h。最佳提取工艺下,提取率为17.15%。
表1正交试验因素水平表
因素水平 | 乙醇浓度 | 料液比 | 提取温度 | 提取时间 |
1 | 60% | 1:10 | 70℃ | 1h |
2 | 70% | 1:12 | 80℃ | 1.5h |
3 | 80% | 1:14 | 90℃ | 2h |
表2正交试验表及结果
试验号 | 乙醇浓度 | 料液比 | 提取温度 | 提取时间 | 提取率(%) |
1 | 1 | 1 | 1 | 1 | 14.52 |
2 | 1 | 2 | 2 | 3 | 16.86 |
3 | 1 | 3 | 3 | 2 | 16.89 |
4 | 2 | 1 | 2 | 2 | 16.91 |
5 | 2 | 2 | 3 | 1 | 16.32 |
6 | 2 | 3 | 1 | 3 | 17.15 |
7 | 3 | 1 | 3 | 3 | 17.08 |
8 | 3 | 2 | 1 | 1 | 16.42 |
9 | 3 | 3 | 2 | 2 | 17.05 |
验证试验根据正交试验结果,以最优工艺重复进行6次验证试验。分别称取薄壳山核桃榨油后的饼粕50g,按照料液比1:14加入70%的乙醇,70℃回流提取2h,提取3次,合并提取液,回收溶剂至无醇味,真空干燥得粗提物,测得的提取率分别为17.12%、17.17%、17.22%、17.19%、17.16%和17.13%,与正交试验相符。测定6次验证试验的粗提物的总酚含量和抗氧化性并计算平均值,结果分别为21.41mg EAE·g-1和127.05μmol TE·g-1。
实施例2总酚含量评价方法
取适量待测样品,加10mL甲醇充分溶解,取10μL酚类物质甲醇液置于10mL离心管中,加入2mL 7.5%的碳酸钠溶液(w/v)、2.5mL 10%的福林酚试剂(v/v),黑暗中50℃水浴反应15min,冷却至室温,紫外760nm处测定吸光值。采用鞣花酸为标准品,绘制标准曲线,结果用每克样品中含有的鞣花酸等价物的量表示(mg Ellagic acid equivalent·g-1,mgEAE·g-1),使用纯甲醇为空白对照。
实施例3同时测定薄壳山核桃中三种酚酸含量的液相色谱方法
色谱条件:流动相:A相,乙腈,B相,2%冰醋酸(v/v),梯度洗脱,0-40min,5-37%A;流速1.0mL·min-1;柱温35℃;进样量10μL;鞣花酸的检测波长为250nm,儿茶素和EGCG的检测波长为280nm。
标准曲线的绘制:准确称取鞣花酸、儿茶素、EGCG三种酚类物质各10mg,用甲醇溶解、定容至10mL,得到1mg·mL-1的单个酚类物质溶液,再分别取三种酚类物质溶液各1mL于10mL容量瓶中,加甲醇定容至10mL配制成含各酚类物质浓度为0.1mg·mL-1的混合标准溶液,逐级稀释2、4、6、8、10倍,进样测定,进样量为10μL。以测定的峰面积为Y值,对应的酚浓度为X值,得标准曲线分别为:鞣花酸y=9766750x+107.65,R2=0.9995;儿茶素y=145650x+1.50,R2=0.9997;EGCG y=537500x+7.75,R2=0.9979。
样品测定:准确称量适量待测样品,加10mL甲醇充分溶解,过0.45μm滤膜后进样测定。结果用每100g样品中各酚类物质的含量(%)表示。
实施例4抗氧化性评价方法
DPPH法:称取39.43mg的DPPH试剂溶于1L甲醇,置于4℃冰箱备用。取适量待测样品,加10mL甲醇充分溶解,取10μL酚类物质甲醇液置于15mL离心管中,加入4mL DPPH甲醇液,黑暗中反应30min,紫外515nm处测定吸光值。采用Trolox为标准品,结果DPPH自由基清除能力(ACDPPH)用每克样品中含有的trolox等价物的量表示(μmol trolox equivalent·g-1,μmol TE·g-1)。使用纯甲醇为空白对照,与样品同时同样方法处理,并从样品中扣去空白吸收值。
实施例5大孔树脂富集工艺优化
大孔树脂富集工艺优化的重点是洗脱溶剂的选择。大孔树脂D101预处理后,水平衡,上样吸附。之后分别采用3BV的水、10%乙醇、20%乙醇、30%乙醇、40%乙醇、50%乙醇、60%乙醇、70%乙醇、80%乙醇、90%乙醇、无水乙醇洗脱,每个极性溶剂冲出的流分分别合并到一起,减压浓缩,真空干燥得提取物,测定提取物的得率、总酚含量和抗氧化性。根据公式:得率(%)=各馏分干样质量(g)/上样干样总质量(g)×100%计算得率,各馏分的得率分别为26.31%、13.16%、9.28%、6.69%、4.56%、3.08%、2.37%、2.64%、1.96%、1.65%和0.95%,总酚含量和抗氧化性结果见图5。从图5中可看出,各馏分中总酚含量和抗氧化性最高的为20%、30%和40%乙醇洗脱的馏分。纯水及10%乙醇得到的馏分得率虽较高,但总酚含量和抗氧化性较低,纯水和10%乙醇洗脱的主要成分为一些大极性的多糖等杂质,50%-无水乙醇部分馏分得率较低且总酚含量和抗氧化性较低,薄壳山核桃中的酚类物质主要集中在20-40%乙醇洗脱馏分部分,因此若拟得到纯度较高且抗氧化性较好的酚类部位应选择性的收集20-40%乙醇洗脱部位。从结果中也可看出,经大孔树脂纯化后总酚含量及抗氧化性均较粗提物大幅度上升。
实施例6
取薄壳山核桃榨油后的饼粕置于提取釜中,按照料液比1:14加入70%的乙醇,70℃回流提取2h,提取3次,合并提取液,回收溶剂至无醇味。上样D101大孔树脂,吸附流速为1BV/h,上样后先用2BV的水洗除杂,水洗脱流速为2BV/h,再用20%和40%的乙醇各2BV洗脱,乙醇洗脱流速为1BV/h,收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚,总酚含量为295.51mg EAE·g-1,鞣花酸含量为6.7%,儿茶素含量为13.4%,EGCG含量为3.7%。
实施例7
取薄壳山核桃榨油后的饼粕置于提取釜中,按照料液比1:14加入70%的乙醇,70度回流提取2h,提取3次,合并提取液,回收溶剂至无醇味。上样AB-8大孔树脂,吸附流速为1BV/h,上样后先用3BV的水洗除杂,水洗脱流速为3BV/h,再用20%和40%的乙醇各2BV洗脱,乙醇洗脱流速为2BV/h,收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚,总酚含量为287.66mg EAE·g-1,鞣花酸含量为6.4%,儿茶素含量为12.8%,EGCG含量为3.5%。
实施例8
取薄壳山核桃榨油后的饼粕置于提取釜中,按照料液比1:14加入70%的乙醇,70℃回流提取2h,提取3次,合并提取液,回收溶剂至无醇味。上样AB-8大孔树脂,吸附流速为1BV/h,上样后先用2BV的水洗除杂,水洗脱流速为2BV/h,再用20%、30%和40%的乙醇各1BV洗脱,乙醇洗脱流速为2BV/h,收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚,总酚含量为315.71mg EAE·g-1,鞣花酸含量为6.9%,儿茶素含量为11.2%,EGCG含量为2.8%。
实施例9
取薄壳山核桃榨油后的饼粕置于提取釜中,按照料液比1:14加入70%的乙醇,70度回流提取2h,提取3次,合并提取液,回收溶剂至无醇味。上样D101大孔树脂,吸附流速为1BV/h,上样后先用3BV的水洗除杂,水洗脱流速为3BV/h,再用20%、30%和40%的乙醇各1BV洗脱,乙醇洗脱流速为2BV/h,收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚,总酚含量为286.97mg EAE·g-1,鞣花酸含量为6.1%,儿茶素含量为11.9%,EGCG含量为2.9%。
实施例10
取薄壳山核桃榨油后的饼粕置于提取釜中,按照料液比1:14加入70%的乙醇,70℃回流提取2h,提取3次,合并提取液,回收溶剂至无醇味。上样D101大孔树脂,吸附流速为1BV/h,上样后先用3BV的水洗除杂,水洗脱流速为3BV/h,再用20%和40%的乙醇各1BV洗脱,乙醇洗脱流速为1BV/h,收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚,总酚含量为269.11mg EAE·g-1,鞣花酸含量为7.1%,儿茶素含量为11.6%,EGCG含量为3.6%。
实施例11
取薄壳山核桃榨油后的饼粕置于提取釜中,按照料液比1:14加入70%的乙醇,70℃回流提取2h,提取3次,合并提取液,回收溶剂至无醇味。上样D101大孔树脂,吸附流速为1BV/h,上样后先用2BV的水洗除杂,水洗脱流速为2BV/h,再用20%、30%和40%的乙醇各2BV洗脱,乙醇洗脱流速为2BV/h,收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚,总酚含量为342.13mg EAE·g-1,鞣花酸含量为6.3%,儿茶素含量为13.6%,EGCG含量为3.5%。
实施例12薄壳山核桃多酚片制备方法
薄壳山核桃总酚提取物10g、甘露醇50g、微晶纤维素25g、羟丙基甲基纤维素10g、微粉硅胶3g、硬脂酸镁2g。将薄壳山核桃总酚提取物与微粉硅胶充分混合,过30目筛,再依次加入甘露醇、微晶纤维素和羟丙基甲基纤维素,混合30min,加入硬脂酸镁混合15min,压片即得。
实施例13薄壳山核桃睡眠面膜制备方法
A相:薄壳山核桃总酚提取物1.8g,溶于无水乙醇380g,65℃搅拌30min。B相:5g卡波姆940,加入甘油50g,搅拌后加水518.2g,搅拌均匀后加入15g吐温80,30g水溶性氮酮,搅拌均匀。将A相趁热边搅拌边加入B相中,搅拌均匀后加入三乙醇胺15mL,搅拌均匀即得睡眠面膜。睡前均匀涂抹于面部,可有效对抗光及污染物给皮肤带来的氧化伤害。
实施例14薄壳山核桃护手霜制备方法
将薄壳山核桃总酚提取物溶解,与适量甜杏仁油、甘油一起加入到180mL纯净水中,加入乳化剂并搅拌,持续加入乳化剂直至形成细腻的霜,加入1mL抗菌剂即得。该护手霜可有效对抗过氧化对皮肤表面的伤害。
Claims (5)
1.一种薄壳山核桃饼粕中具有抗氧化活性酚类物质的制备方法,其特征在于,包括以下步骤:
(1) 取薄壳山核桃榨油后的饼粕,加入乙醇回流提取1-3次,合并提取液,回收溶剂至无醇味;
(2) 提取液采用大孔树脂纯化,提取液吸附流速为1BV/h,上样后先用2-3BV的水洗除杂,水洗脱流速为2-3 BV/h,再用乙醇洗脱,乙醇用量为2-4BV,乙醇洗脱流速为1-2 BV/h;
(3) 收集乙醇洗脱液,减压回收溶剂至小体积,真空干燥,即得薄壳山核桃总多酚。
2.根据权利要求1所述的制备方法,其特征在于步骤(1)中乙醇浓度为50-90%,料液比为1:10-18,提取温度为60-90℃,提取时间为1-3h,提取3次。
3.根据权利要求1所述的制备方法,其特征在于步骤(2)中所用的大孔树脂型号为D101或AB-8,洗脱乙醇浓度为20-40%。
4.根据权利要求1所述的制备方法,其特征在于步骤(3)中所获得的薄壳山核桃总多酚,其总酚含量为200-400mg EAE•g−1,其中按质量百分比计,鞣花酸含量为5-8%,儿茶素含量为10-15%,EGCG含量为2-5%。
5.根据权利要求1所述方法获得的薄壳山核桃总多酚在制备具有抗氧化功效的保健品和化妆品中的应用。
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