CN105434478A - 一种海嵩子多酚的制备方法 - Google Patents
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Abstract
本发明提供了一种海嵩子多酚的制备方法,海嵩子干与20倍体积分数的40%乙醇溶液均匀混合、30℃水浴浸提46min,4000r/min浸提液离心10min,重复浸提2次,得多酚提取液;本发明利用响应面法优化海嵩子多酚最佳提取条件的方法,设置乙醇的体积分数、料液比和浸提时间3个自变量;利用Box-Benhnken响应面设计的原则进行筛选;采用Design?expert软件进行实验设计和结果分析;本发明提供的海嵩子多酚的提取工艺提高了多酚的提取率,对于多酚的工业化生产具有重要作用。
Description
技术领域
本发明涉及功能性食品或生物医药领域,具体涉及一种海嵩子多酚的制备方法。
背景技术
海蒿子SargassumconfusumC.Ag.是生长在暖温带水域的植物,我国沿海资源丰富。海嵩子富含生物活性物质,具有很高的保健和药用价值。海蒿子多糖对白血病细胞株有毒副作用,可抑制肿瘤细胞的增殖。褐藻糖胶也是主要的活性成分之一,现代研究表明,褐藻糖胶具有抗肿瘤、抗病毒、抗血栓、抗氧化、调节血脂、抗辐射和抑制补体激活等多种生理功能。我国海嵩子资源丰富,但由于对海嵩子综合开发的研究起步较晚,对其生物活性的研究也大多集中在海嵩子多糖,对海嵩子多酚的未见报道。
多酚(Phlorotannins)是一类结构独特的天然化合物,其基本结构单元是间苯三酚,具有抑菌、抗凝血、降血脂、抗肿瘤、抗氧化等生物活性功能。根据其特有的抗氧化活性提取海嵩子多酚进行加工,从而开发功能性产品如抗氧化剂,具有很广阔的市场前景。褐藻类在我国沿海品种纷繁的经济资源中占据显著地位,是我国三大经济海藻之一,海嵩子多酚的提取制备技术研究对于充分开发海藻资源具有重要意见,为海嵩子多酚功能性产品开发提供一定的理论依据和技术指导,为拓展海嵩子深加工产品领域提供一条有效途径。
海嵩子的干燥,如采取传统的干燥方法包括晒干、烘干、晾干、微波干燥和冷冻干燥。然而几种方法并不适于海嵩子的干燥。烘干、晾干和微波干燥易造成海嵩子中多酚的损失;海嵩子在晾干过程因为表面微生物多干燥速度慢,容易腐败变质;冷冻干燥存在处理速度慢、成本高等问题,无法普及使用。
微波辅助提取、超声辅助提取,可以缩短浸提时间,提取率高,操作简便,提取结构不易破坏,但成本高、能耗大,目前普遍采用的提取多酚的方法为有机溶剂浸提法。影响海嵩子多酚提取的因素还有溶剂体积分数、液料比、浸提温度、浸提时间、浸提次数等,原材料的前处理也影响多酚物质的浸出,然而目前采用传统实验设计方法进行海嵩子多酚的提取工艺存在实验次数多,实验耗时长、海嵩子多酚提取率低、人力物力投入较大等不足,不利于工业化生产。
发明内容
本发明的目的在于针对现有技术的不足,提供一种海嵩子多酚的制备方法,具体为一种保护海嵩子中多酚干燥过程免受破坏,干燥速度较快,先以电解水对海嵩子表面减菌处理,再以酒精消毒进一步减少海嵩子表面的微生物,以滚筒辗压破坏海嵩子紧密结构利于水分析出增加干燥速度,再辅以分段烘干,可以较快速度干燥海嵩子又不容易腐败。同时本发明以较少的实验次数和较短的时间对所选实验参数进行全面分析的实验设计从而获得的海嵩子多酚的提取工艺。
为了实现上述目的,本发明采取的技术方案如下:
(1)先用洁净海水把采集的新鲜海嵩子表面的杂质和沙粒冲洗干净,电解水浸泡淡化和减菌,再用75%酒精浸烫泡消毒3-5S,沥干。
(2)海嵩子摊铺于瓷盘,厚2cm-4cm,用滚筒轻轻碾压3-5min,以海嵩子成蔫状、不出汁为宜。
(3)置冷风干燥箱,调整温度20-30℃,风速2-5m/s,湿度40%以下,冷风干燥至水分含量低于12-15%;调整温度至5-10℃,风速2-5m/s,湿度30%以下,冷风干燥至水分含量低于6%以下。
(4)用粉碎机将干海嵩子粉碎成粗粉,然后用振动式药物超微粉碎机在-10℃条件下粉碎8-15min,真空密封,-18℃、避光贮藏备用。
(5)称取干燥的海嵩子粉末于10mL离心管中,与0%~95%乙醇溶液以1:5~30的料液比均匀混合,浸提20~120min,隔3~6min振荡一次。
(6)冷却后,4000r/min离心8~12min,将上清液转移至容量瓶。
(7)残渣再用0%~95%乙醇溶液提取一次,重复浸提1~3次,合并提取液定容到10mL;
(8)利用响应面法设计筛选出海嵩子多酚的最优提取工艺,对浸提液体积分数,浸提时间,料液比三个影响海嵩子多酚提取过程的关键因素进行三因素三水平的实验设计,得到的最佳的提取工艺为:将海嵩子粉末与40%乙醇溶液以1:20的料液体积比均匀混合,在30℃水浴中浸提46min,隔4min振荡一次,4000r/min浸提液离心10min,将上清液转移至容量瓶;残渣再用40%乙醇溶液提取一次,重复浸提2次;合并提取液,得海嵩子多酚提取液,海嵩子多酚的得率为1.304%。
所述的筛选方法是采用Box-Benhnken响应面设计法优化海嵩子多酚最佳提取工艺的方法。相比正交试验要进行33组实验,响应面法只需要进行15组实验对海嵩子多酚的提取条件乙醇浓度、提取时间、料液比3个因素进行优化,获得了最佳的提取工艺及提取率,提高了提取效率和海嵩子原料的利用率,对于海嵩子多酚的工业化生产和应用具有实际的意义。
海嵩子综上所述,本发明采用的Box-Benhnken响应面设计法比传统的正交设计法相比,对3个影响因子进行三水平,以更少的实验次数就可得到结果,大大缩短了实验时间,节约了经济和人力成本。通过响应面设计优化乙醇浓度、提取时间和料液比的最优组合,得到了海嵩子多酚最佳的提取工艺。
具体实施方式
结合具体实施例进行说明。
实施例1。
一、通过以下步骤进行海嵩子多酚的提取和含量测定。
1、样品准备和前处理:先用洁净海水把采集的新鲜海嵩子表面的杂质和沙粒冲洗干净,电解水浸泡淡化和减菌,再用75%酒精浸烫泡消毒3-5S,沥干。海嵩子摊铺于瓷盘,厚2cm-4cm,用滚筒轻轻碾压3-5min,以海嵩子成蔫状、不出汁为宜。置冷风干燥箱,调整温度20-30℃,风速2-5m/s,湿度40%以下,冷风干燥至水分含量低于12-15%;调整温度至5-10℃,风速2-5m/s,湿度30%以下,冷风干燥至水分含量低于6%以下。粉碎备用。
2、称取干燥的海嵩子粉末0.2g于10mL离心管中,与在10~30℃的0%~95%乙醇溶液以1:5~30的料液比均匀混合,在30℃水浴中浸提20~120min,隔3~6min振荡一次,冷却后,4000r/min离心8~12min,将上清液转移至容量瓶。残渣再用0%~95%乙醇溶液提取一次,重复浸提1~3次,合并提取液定容到10mL,然后按一定稀释倍数稀释,采用福林酚法,采用茶多酚国家标准GB/T8313-2008测定海嵩子多酚含量,即以没食子酸作为标准品,在765nm波长条件下用分光光度计测其吸光度值(A)。以吸光度为纵坐标,没食子酸的浓度(μg/mL)为横坐标,绘制标准曲线,测定样品的吸光度,计算海嵩子多酚产品的产率。
3、计算海嵩子多酚得率,得率(%)=[A×V×d]/[k×M×106×m]×100%,其中,A为在765nm波长条件下海嵩子多酚提取液的吸光值;V为提取液体积;d为稀释因子;k为没食子酸标准曲线的斜率;M为样品干物质的含量(%);m为海嵩子的质量(g)。
二、实验设计及统计学方差分析。
1、单因素实验设计。
通过改变提取液乙醇的体积分数、提取时间、提取温度、料液比、浸提次数进行单因素实验,根据GB/T8313-2008多酚测定国家标准测定海嵩子多酚含量,每次处理进行3次重复实验。
2、响应面实验设计。
在单因素实验的基础上,选取乙醇体积分数(%),浸提时间(min),液料比(mL/g)三个影响海嵩子多酚提取率的关键因素,以海嵩子多酚的提取率(%)为响应值,进行响应面法优化海嵩子多酚提取工艺,利用DesignExpert8.0.6软件进行数据拟合和分析,实验因素和水平见表1。
表1响应面设计因素和水平设定表
以乙醇体积分数(%),浸提时间(min),液料比(mL/g)三个影响海嵩子多酚提取率的关键因素因素,以海嵩子多酚的提取率(%)为响应值,进行Box-Benhnken响应面实验,实验设计和结果见表2。
表2Box-Behnken响应面试验方案及结果。
3、响应面预测模型的建立及模型方差分析。
利用DesignExpert8.0.6软件对表2响应面分析方案和结果数据进行多元回归拟合,获得海嵩子多酚提取率(Y)对自变量溶剂浓度(A)、提取时间(B)、液料比(C)的二次多项回归模型方程:提取率Y=-0.125+0.094A+0.031B+0.144C+3×10-5AB-5.875×10-4AC+2.475×10-4BC-1.049×10-3A2-3.960×10-4B2-2.947×10-3C2。
P水平是检验回归系数的标准,当P<0.05时表明回归方程显著;当P<0.01时表明回归方程高度显著;当P>0.05时表明回归方程不显著。对海嵩子多酚的响应面分析方案和结果数据进行方差分析,表明用此模型对海嵩子多酚提取工艺结果进行很好的分析和预测。
对响应面法优化得到的回归模型进行分析,海嵩子多酚的最优的浸提条件为:乙醇浓度为40%,浸提时间46min,液料比20:1,在此条件下,模型预测理论浸出率最大值为1.317%。
实施例2.
一种海嵩子多酚提取方法,包含以下步骤:
海嵩子冲洗干净,电解水浸泡淡化和减菌,再用75%酒精浸烫泡消毒4S,沥干。海嵩子摊铺于瓷盘,厚3cm,用滚筒轻轻碾压5min,以海嵩子成蔫状、不出汁为宜。置冷风干燥箱,调整温度25℃,风速2m/s,湿度40%,冷风干燥至水分含量12%;调整温度至10℃,风速2m/s,湿度30%,冷风干燥至水分含量6%。用粉碎机将干海嵩子粉碎成粗粉,然后用振动式药物超微粉碎机在-10℃条件下粉碎12min,得海嵩子粉末。取上述海嵩子粉末加20倍体积分数为40%乙醇溶液(即料液比1:20)、在30℃水浴中浸提46min,浸提液4000r/min离心10min,将上清液转移至容量瓶。残渣再用40%乙醇甲醇溶液提取一次,重复浸提2次,合并提取液定容到10mL,然后按一定稀释倍数稀释;提取液以福林酚法测定多酚含量,多酚得率为1.312%。
Claims (3)
1.一种海嵩子多酚的制备方法,其特征在于:所述方法为将干燥的海嵩子粉末与0%~95%乙醇溶液以1:5~30的料液体积比均匀混合,浸提20~120min,隔3~6min振荡一次;冷却后,4000r/min离心8~12min,将上清液转移至容量瓶;残渣再用0%~95%乙醇溶液提取一次,重复浸提1~3次,合并提取液。
2.据权利要求1所述的一种海嵩子多酚的制备方法,其特征在于:海嵩子粉末的制备方法具体为:
(1)先用洁净海水把采集的新鲜海嵩子表面的杂质和沙粒冲洗干净,电解水浸泡淡化和减菌,再用75%酒精浸烫泡消毒3-5S,沥干;
(2)海嵩子摊铺于瓷盘,厚2cm-4cm,用滚筒轻轻碾压3-5min,以海嵩子成蔫状、不出汁为宜;
(3)置冷风干燥箱,调整温度20-30℃,风速2-5m/s,湿度40%以下,冷风干燥至水分含量低于12-15%;调整温度至5-10℃,风速2-5m/s,湿度30%以下,冷风干燥至水分含量低于6%以下;
(4)用粉碎机将干海嵩子粉碎成粗粉,然后用振动式药物超微粉碎机在-10℃条件下粉碎8-15min,粉碎过80目筛,真空密封,-18℃、避光贮藏备用。
3.据权利要求1所述的海嵩子多酚的提取方法,其特征在于:将海嵩子粉末与40%乙醇溶液以1:20的料液比均匀混合,在30℃水浴中浸提46min,隔4min振荡一次,4000r/min浸提液离心10min,将上清液转移至容量瓶;残渣再用40%乙醇溶液提取一次,重复浸提2次;合并提取液,得海嵩子多酚提取液。
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