CN109529784A - 多酚等梯度吸附纳米复合物及其制备方法 - Google Patents
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Abstract
本发明属于食品添加剂和生物药剂复合制备领域,具体涉及一种多酚等梯度吸附纳米复合物及其制备方法。包括下述步骤:1)磺化纳米纤维素母液的配置:2)磺化纳米纤维素吸附多酚的复合物稀乳液的制备;3)将步骤2)得到的磺化纳米纤维素‑多酚抗氧化复合物制备成乳液、粉末或者颗粒产品。本发明使用全新的磺化纳米纤维素能够能先等梯度的多酚吸附。
Description
技术领域
本发明属于食品添加剂和生物药剂复合制备领域,具体涉及一种多酚等梯度吸附纳米复合物及其制备方法。
背景技术
多酚类物质作为天然抗氧化剂的一种,主要活性成分为多酚类物质,其具有很强抗氧化作用,它可以去除体内自由基,保证身体活力延缓衰老,被称为“第七类营养素。它普遍存在于常见的植物性食物,如可可豆、大豆、水果、蔬菜、谷物和茶叶等中。由于其极高的保健功效,而深受食品行业的欢迎。。
对于食品行业而言,多酚类物质的强抗氧化性能够有效中断脂肪氧化的链式反应,抑制氧化产物的生成,可以作为抗氧化剂广泛应用于肉制品加工、油脂储藏、乳制品、烘焙制品及干鱼制品中。多酚类物质本身还具有很强的抑菌性,对于普通的肉毒杆菌、金葡球菌、变性杆菌等都有一定的抑制和杀伤作用,是一类公认的强效、低毒性抗菌产品。此外,多酚类物质可以减缓摘后果蔬的生化活动,能有效的防止叶绿色、胭脂红、维生素等天然色素因光照而褪色,从而延长储藏时间。
而对于生物制药行业而言,多酚类物质拥有预防胃癌、肠癌等肿瘤疾病心以及动脉粥样硬化等血管疾病的作用,可以清除因紫外线诱导生成的自由基,从而保护黑色素细胞正常功能,起到美白的作用。多酚类物质的理疗作用,包括控制肠道的菌群、改善调节肠道内环境,以及抗毒、消炎抗过敏等功效也均已被大量科研试验所证明。
目前,对于多酚类物质的分离吸附主要有化学吸附和物理吸附方式,物理吸附主要包括活性炭吸附,沸石吸附,离子交换吸附和大孔树脂吸附,如专利号201310290155.9,201410322591.4采用大孔树脂对多酚类物质的吸附方法。化学吸附主要利用对吸附材料的改性实现对多酚类物质的吸附,如申请号201710702658.0利用乙烯基苯硼酸接枝到纤维素分子链上,利用苯硼酸与多酚中的邻苯二酚结构在碱性条件下可以生成硼酸酯,在酸性条件下硼酸酯发生解离的机理,实现多酚的吸附和解离;但上述方法所得到的复合物却难以实现等梯度吸附。
发明内容
本发明的目的在于提供一种多酚等梯度吸附纳米复合物及其制备方法。
本发明为实现上述目的,采用以下技术方案:
一种多酚等梯度吸附纳米复合物的制备方法,包括下述步骤:
1)磺化纳米纤维素母液的配置:
1a)磺化纳米纤维素粉末的制备如式(I)示出:具体包括将棉粉或者溶解浆配置成15-17wt%的浆液,与硫酸盐酸混合液在40°条件下反应1.5-2h,反应结束后对产物进行离心或者透析清洗至pH为中性;对产物进行冷冻干燥后粉碎得到磺化纳米纤维素粉末;其中,棉粉或溶解浆与硫酸盐酸混合液的重量比例为17:100;
1b)纳米纤维素磺化母液的制备:将3-3.5质量份磺化纳米纤维素粉末加入90-92质量份的去离子水,得到胶体溶液,之后加入增稠剂壳聚糖,在恒温冰水浴条件下利用均质机进行预剪切,得到粘度为260mPa·s-300mPa·s的基材母液;
2)磺化纳米纤维素吸附多酚的复合物稀乳液的制备:
按多酚与有机溶剂的质量比为1:2进行混合,在超声条件下,使多酚完全溶解得到多酚溶液;在6000r/min~10000r/min转速下,向通过步骤1b)所得到的基材母液中逐滴滴加多酚溶液;待多酚溶液滴加结束后,提高转速至18000r/min~20000r/min,使多酚分子有效吸附于磺化纳米纤维素的表面,从而制得高稳定性单层吸附模式的磺化纳米纤维素-多酚抗氧化复合物;
3)将步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物制备成乳液、粉末或者颗粒产品。
具体的,步骤1)中所述的硫酸盐酸混合液为68.5wt%的硫酸与15.5wt%的盐酸按照质量比为3:1制得。
步骤1b)中均质机的转速为6000r/min-8000r/min;剪切时间为25min~35min;壳聚糖的数均分子量为25000~48000。
优选的,步骤1b)中均质机的转速为7000r/min;剪切时间为30min。
步骤2)中的超声条件为:80-100KHZ。
步骤3)中乳液的制备方法:经步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物通过真空旋转蒸发器进行浓缩,得到多酚活性组分对乳液总量的绝干比重为50%-75%的产品乳液。
所述的真空旋转蒸发器的浓缩条件为真空度<-0.08MPa,温度30℃-36℃。
步骤3)中颗粒的制备方法为将产品乳液真空冷冻干燥后,再经超微粒粉碎机处理,得到粒度为0.25μm-6μm的磺化纳米纤维素-多酚复合物固体颗粒。
步骤3)中粉末的制备方法为将产品乳液经过喷雾干燥,得到粒径为0.1μm-7μm的固体粉末产品。
本发明还包括一种多酚等梯度吸附纳米复合物,采用所述的制备方法得到。
与现有技术相比,本发明的有益效果是:
本发明使用全新的磺化纳米纤维素从而实现对多酚的等梯度吸附。从技术原理层面上讲,由于磺酸基对于纳米纤维素C6位活泼羟基的替代,剩余的吸附活性接近的C2和C3位羟基可以以等速率实现对多酚的吸附。此外,在制备过程中所使用的恒温剪切法可以保证多酚在磺化纳米纤维素颗粒表面等梯度吸附。
具体实施方式
为了使本技术领域的技术人员更好地理解本发明的技术方案,下面结合最佳实施例对本发明作进一步的详细说明。
实施例1:
一种多酚等梯度吸附纳米复合物乳液的制备方法,包括下述步骤:
1)纳米纤维素磺化母液的配置:
1a)纳米纤维素磺化粉末的制备:具体包括将棉粉配置成16wt%的浆液,与硫酸盐酸混合液在40°条件下反应1.7h,反应结束后对产物进行离心或者透析清洗至pH为中性;对产物进行冷冻干燥后粉碎得到磺化纳米纤维素粉末;其中,棉粉与硫酸盐酸混合液的重量比例为17:100;所述的硫酸盐酸混合液为68.5wt%的硫酸与15.5wt%的盐酸按照质量比为3:1制得。
1b)纳米纤维素磺化母液的制备:将3.2质量份磺化纳米纤维素粉末加入91质量份的去离子水,得到胶体溶液,之后加入增稠剂壳聚糖,壳聚糖的数均分子量为30000。在恒温冰水浴条件下利用均质机进行预剪切,均质机的转速为7000r/min;剪切时间为30min,得到粘度为280mPa·s的基材母液;
2)磺化纳米纤维素吸附多酚的复合物稀乳液的制备:
按多酚与有机溶剂的质量比为1:2进行混合,在超声条件(90KHZ)下,使多酚完全溶解得到多酚溶液;在7000r/min转速下,向步骤1b)得到的基材母液中逐滴滴加多酚溶液;待多酚溶液滴加结束后,提高转速至19000r/min,使多酚分子有效吸附于磺化纳米纤维素的表面,从而制得高稳定性单层吸附模式的磺化纳米纤维素-多酚抗氧化复合物;
3)将步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物通过真空旋转蒸发器进行浓缩,得到多酚活性组分对乳液总量的绝干比重为50%-75%的产品乳液。
对上述复合乳液离心处理后,对上清液进行总酚含量测定,以确定多酚在磺化纳米纤维素表面的吸附率。取6支试管,每只试管分别加入0、0.1、0.2、0.3、0.4、0.5ml的没食子酸标准样品,再加入0.7ml福林酚试剂、3ml7.5%的碳酸钠,混匀静置5min。经过75℃水浴处理10min后,立即将溶液至于冰浴中冷却并离心。离心操作条件设置为转速为5000r/min,温度4℃,离心处理时间5min。取上清液于730nm波长下测定吸光度的值,并根据没食子酸溶液的浓度和吸光度值,绘制标准曲线。然后吸取0.5ml测试样品于试管中,福林试剂和碳酸钠浓度、反应温度及反应时间均按照上述条件设定,根据标准曲线公式计算样品中残余多酚的含量,进而计算被吸附的多酚含量。测试结果表明本实施例所制得的纳米抗氧化复合物在本发明所设定的恒温剪切条件下可以实现等梯度吸附,吸附速率为7.75-8.25%/10min。
实施例2:
一种多酚等梯度吸附纳米复合物颗粒的制备方法,包括下述步骤:
1)纳米纤维素磺化母液的配置:
1a)纳米纤维素磺化粉末的制备:具体包括将溶解浆配置成15wt%的浆液,与硫酸盐酸混合液在40°条件下反应1.5h,反应结束后对产物进行离心或者透析清洗至pH为中性;对产物进行冷冻干燥后粉碎得到磺化纳米纤维素粉末;其中,溶解浆与硫酸盐酸混合液的重量比例为17:100;所述的硫酸盐酸混合液为68.5wt%的硫酸与15.5wt%的盐酸按照质量比为3:1制得。
1b)纳米纤维素磺化母液的制备:将3质量份磺化纳米纤维素粉末加入90质量份的去离子水,得到胶体溶液,之后加入增稠剂壳聚糖,壳聚糖的数均分子量为25000。在恒温冰水浴条件下利用均质机进行预剪切,均质机的转速为6000r/min;剪切时间为35min;得到粘度为260mPa·s的基材母液;
2)磺化纳米纤维素吸附多酚的复合物稀乳液的制备:
按多酚与有机溶剂的质量比为1:2进行混合,在超声条件(80KHZ)下,使多酚完全溶解得到多酚溶液;在6000r/min转速下,向步骤1b)得到的基材母液中逐滴滴加多酚溶液;待多酚溶液滴加结束后,提高转速至18000r/min,使多酚分子有效吸附于磺化纳米纤维素的表面,从而制得高稳定性单层吸附模式的磺化纳米纤维素-多酚抗氧化复合物;
3)将步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物制备成颗粒产品;将步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物通过真空旋转蒸发器进行浓缩,得到多酚活性组分对乳液总量的绝干比重为50%-75%的产品乳液。所述的真空旋转蒸发器的浓缩条件为真空度<-0.08MPa,温度30℃-36℃。将产品乳液真空冷冻干燥后,再经超微粒粉碎机处理,得到粒度为0.25μm-6μm的磺化纳米纤维素-多酚复合物固体颗粒。
实施例2与实施例1所使用的绘制标准曲线的方法相同。然后称取5g测试样品于试管中,福林试剂和碳酸钠浓度、反应温度及反应时间均按照上述条件设定,根据标准曲线公式计算样品中残余多酚的含量,进而计算被吸附的多酚含量。测试结果表明本实施例所制得的纳米抗氧化复合物在本发明所设定的恒温剪切条件下可以实现等梯度吸附,吸附速率为7.25-7.5%/10min。
实施例3:
一种多酚等梯度吸附纳米复合物粉末的制备方法,包括下述步骤:
1)纳米纤维素磺化母液的配置:
1a)纳米纤维素磺化粉末的制备:具体包括将棉粉配置成17wt%的浆液,与硫酸盐酸混合液在40°条件下反1.5-2h,反应结束后对产物进行离心或者透析清洗至pH为中性;对产物进行冷冻干燥后粉碎得到磺化纳米纤维素粉末;其中,棉粉与硫酸盐酸混合液的重量比例为17:100;所述的硫酸盐酸混合液为68.5wt%的硫酸与15.5wt%的盐酸按照质量比为3:1制得。
1b)纳米纤维素磺化母液的制备:将3.5质量份磺化纳米纤维素粉末加入92质量份的去离子水,得到胶体溶液,之后加入增稠剂壳聚糖,壳聚糖的数均分子量为48000,在恒温冰水浴条件下利用均质机进行预剪切,得到粘度为300mPa·s的基材母液;均质机的转速为8000r/min;剪切时间为25min;得到粘度为260mPa·s的基材母液;
2)磺化纳米纤维素吸附多酚的复合物稀乳液的制备:
按多酚与有机溶剂的质量比为1:2进行混合,在超声条件下,使多酚完全溶解得到多酚溶液;10000r/min转速下,向步骤1b)得到的基材母液中逐滴滴加多酚溶液;待多酚溶液滴加结束后,提高转速至20000r/min,使多酚分子有效吸附于磺化纳米纤维素的表面,从而制得高稳定性单层吸附模式的磺化纳米纤维素-多酚抗氧化复合物;
3)将步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物制备成粉末产品;经步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物通过真空旋转蒸发器进行浓缩,得到多酚活性组分对乳液总量的绝干比重为50%-75%的产品乳液。所述的真空旋转蒸发器的浓缩条件为真空度<-0.08MPa,温度30℃-36℃。将产品乳液经过喷雾干燥,得到粒径为0.1μm-7μm的固体粉末产品。
实施例3与实施例1所使用的绘制标准曲线的方法相同。然后称取5g测试样品于试管中,福林试剂和碳酸钠浓度、反应温度及反应时间均按照上述条件设定,根据标准曲线公式计算样品中残余多酚的含量,进而计算被吸附的多酚含量。测试结果表明本实施例所制得的纳米抗氧化复合物在本发明所设定的恒温剪切条件下可以实现等梯度吸附,吸附速率为7.05-7.6%/10min。
以上内容仅为本发明的较佳实施例,对于本领域的普通技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处,本说明书内容不应理解为对本发明的限制。
Claims (10)
1.一种多酚等梯度吸附纳米复合物的制备方法,其特征在于,包括下述步骤:
1)磺化纳米纤维素母液的配置:
1a)磺化纳米纤维素-粉末的制备如式(I)示出:具体包括将棉粉或者溶解浆配置成15-17wt%的浆液,与硫酸盐酸混合液在40°条件下反应1.5-2h,反应结束后对产物进行离心或者透析清洗至pH为中性;对产物进行冷冻干燥后粉碎得到磺化纳米纤维素粉末;其中,棉粉或者溶解浆与硫酸盐酸混合液的重量比例为17:100;
1b)纳米纤维素磺化母液的制备:将3-3.5质量份磺化纳米纤维素粉末加入90-92质量份的去离子水,得到胶体溶液,之后加入增稠剂壳聚糖,在恒温冰水浴条件下利用均质机进行预剪切,得到粘度为260mPa·s-300mPa·s的基材母液;
2)磺化纳米纤维素吸附多酚的复合物稀乳液的制备:
按多酚与有机溶剂的质量比为1:2进行混合,在超声条件下,使多酚完全溶解得到多酚溶液;在6000r/min-10000r/min转速下,向通过步骤1b)所得到的基材母液中逐滴滴加多酚溶液;待多酚溶液滴加结束后,提高转速至18000r/min-20000r/min,使多酚分子有效吸附于磺化纳米纤维素的表面,从而制得高稳定性单层吸附模式的磺化纳米纤维素-多酚抗氧化复合物;
3)将步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物制备成乳液、粉末或者颗粒产品。
2.根据权利要求1所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤1)中所述的硫酸盐酸混合液为68.5wt%的硫酸与15.5wt%的盐酸按照质量比为3:1制得。
3.根据权利要求1所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤1b)中均质机的转速为6000r/min-8000r/min;剪切时间为25min~35min;壳聚糖的数均分子量为25000~48000。
4.根据权利要求1所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤1b)中均质机的转速为7000r/min;剪切时间为30min。
5.根据权利要求1所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤2)中的超声条件为:80-100KHZ。
6.根据权利要求1所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤3)中乳液的制备方法:经步骤2)得到的磺化纳米纤维素-多酚抗氧化复合物通过真空旋转蒸发器进行浓缩,得到多酚活性组分对乳液总量的绝干比重为50%-75%的产品乳液。
7.根据权利要求6所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,所述的真空旋转蒸发器的浓缩条件为真空度<-0.08MPa,温度30℃-36℃。
8.根据权利要求6所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤3)中颗粒的制备方法为将产品乳液真空冷冻干燥后,再经超微粒粉碎机处理,得到粒度为0.25μm-6μm的磺化纳米纤维素-多酚复合物固体颗粒。
9.根据权利要求6所述的多酚等梯度吸附纳米复合物的制备方法,其特征在于,步骤3)中粉末的制备方法为将产品乳液经过喷雾干燥,得到粒径为0.1μm-7μm的固体粉末产品。
10.一种多酚等梯度吸附纳米复合物,其特征在于,采用权利要求1-9任一项所述的制备方法得到。
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