CN115089729A - 一种β-环糊精类紫甘薯花青素微胶囊的制备方法 - Google Patents
一种β-环糊精类紫甘薯花青素微胶囊的制备方法 Download PDFInfo
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- CN115089729A CN115089729A CN202210751474.4A CN202210751474A CN115089729A CN 115089729 A CN115089729 A CN 115089729A CN 202210751474 A CN202210751474 A CN 202210751474A CN 115089729 A CN115089729 A CN 115089729A
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Abstract
本发明公开了一种β‑环糊精类紫甘薯花青素微胶囊的制备方法,选择β‑环糊精、β‑环糊精衍生物为囊材,以经提取和纯化得到的纯净紫甘薯花青素为芯材,将囊材和芯材在pH 2.6~3.0的缓冲体系中混匀,并经过超声及磁力搅拌使其充分作用后进行真空冷冻干燥,制得的紫甘薯花青素微胶囊能有效提高紫甘薯花青素的稳定性,便于紫甘薯花青素的运输、储存和使用。
Description
技术领域
本发明涉及紫甘薯花青素的制剂开发,尤其涉及一种紫甘薯花青素微胶囊的制备方法。
背景技术
紫甘薯,别名紫薯,块根及茎叶中富含花青素,有望成为食品、药品中花青素的主要来源。有研究表明,紫甘薯花青素的主要成分为矢车菊素和芍药素以及少量的天竺葵色素,其以糖苷化后的酰基化衍生物形式存在,具有抗氧化、抗突变、抗肿瘤等多种功能,可以用于预防癌症、心血管疾病及肥胖等多种疾病。
紫甘薯花青素对温度、pH、光照、氧气、金属离子和酶等环境和化学因素高度敏感,限制了其在实际生产中的广泛应用。因此改善花青素的稳定性对扩大其应用范围十分必要。微胶囊化是防止花青素降解、提高其稳定性的一种有效且实用的方法。它是通过囊材包衣目标物以形成微米或纳米级胶囊,可以保护囊腔内目标物不受环境影响,以延长储存期限;改变目标物的存在状态,以便于储存及运输;掩盖目标物的不良气味,以提高产品可接受度;以及提高目标物中的活性化合物的生物利用度以及控制其释放。近年来,随着微胶囊技术的研究不断深入,除了传统的药物微胶囊外,微胶囊已逐渐扩展到食品、化妆品及保健品等诸多领域。
目前,国内外制备花青素微胶囊的方法主要有喷雾干燥法、冷冻干燥法、相分离法和复凝聚法等,其中喷雾干燥法生产效率高、操作简单,但是由于喷雾干燥过程需要高温辅助,故易破坏温度敏感型物质,从而导致花青素的保留率低。冷冻干燥法干燥后的物料能保持原来的化学组成和物理性质,因此适用于温度敏感型物质,采用冷冻干燥法制备的微胶囊显示出较高的收率和花青素保留率。
β-环糊精(β-CD)是制药、食品和化妆品制造业中良好的稳定剂和调味剂,主要用于提高物质的稳定性、乳化能力和防潮能力,防止其氧化和分解。Fernandes等研究了矢车菊素-3-O-葡萄糖苷和β-CD的分子包合作用,结果表明,通过将矢车菊素-3-O-葡萄糖苷与β-CD按大约1:10的比例(w:w)混合,并经搅拌、冷冻干燥制备分子包合物,可以增加黑莓花青素的热稳定性,并降低其在模拟胃液中的降解速率,从而提高了花青素的生物利用度(Fernandes A,Rocha MAA,Santos LMNB,et al.Blackberry anthocyanins:β-Cyclodextrin fortification for thermal and gastrointestinalstabilization.Food Chemistry,2018,245:426-431.),但该文献并未考察包埋率。
为了提高β-环糊精对微胶囊芯材的包合效果,可以对相应的包合工艺进行优化。在中国专利CN103251570A中对β-环糊精-艾地苯醌混合溶液进行超声包合,包合溶液经静置后抽滤、干燥,再经磨细、过筛,解决了艾地苯醌的水溶性问题;在中国专利CN102342471A中将β-环糊精与白豆蔻挥发油经均质所得乳液超声,再冷藏、抽滤、冷冻干燥,获得白豆蔻挥发油微胶囊产品,解决了白豆蔻挥发油保存时间短的问题。尽管后一专利通过乳化提高了包埋率,但并不适合对水溶性成分的包合,而前一专利则是围绕水不溶性芯材的包合率进行工艺优化。
微胶囊囊材的性质也是影响包埋效果和维持稳定的重要因素。鉴于花青素的环境敏感性和基于对抗氧化活性的保护,寻找β-环糊精之外的具备良好的包埋效率及产率的囊材,对于发挥微胶囊的作用具有重要意义。Wilkowska等将羟丙基-β-环糊精与高浓度蓝莓花色苷混合后加入吐温80作为乳化剂进行均质化,再经喷雾干燥制得喷雾干燥粉;同时将β-环糊精与高浓度蓝莓花色苷混合后,经搅拌、冷冻干燥制得冻干粉;结果表明,在喷雾干燥过程中,总酚类物质的损失平均达76%~78%,而花青素的损失约为57%,冻干粉对花青素的保留率较高,约为喷雾干燥粉的1.5倍(Wilkowska A,Ambroziak W,A,etal.Effect of microencapsulation by spray drying and freeze-drying techniqueon the antioxidant properties of blueberry(vaccinium myrtillus)juicepolyphenolic compounds.Polish Journal of Food and Nutrition Sciences,2016,66(1):11-16.),但该文献并未考察包埋率。Milea等以乳蛋白及其水解产物和β-环糊精为囊材,采用冷冻干燥法和分子包囊法对黑米和薰衣草中的生物活性物质进行微胶囊化研究,结果表明,花色素苷的包埋率约为99%,精油的包埋率约为65.5%,所得混合微胶囊具有良好的稳定性和自由基清除活性,并能预防糖尿病的发生(Milea SA,Dima CV,Enachi E,etal.Combination of freeze drying and molecular inclusion techniques improvesthe bioaccessibility of microencapsulated anthocyanins from black rice(Oryzasativa L.)and lavender(Lavandula angustifolia L.)essential oils in a modelfood system.International Journal of Food Science&Technology,2020,55(12):3585-3594;包埋率译名参考“崔丽霞.紫苏花色苷提取纯化及其微胶囊化研究.太原:中北大学,2018.”),但该文献并未考察稳定性。
发明内容
本发明的目的在于提供一种β-环糊精类紫甘薯花青素微胶囊的制备方法,从而能够通过充分发挥微胶囊化对水溶性活性物质紫甘薯花青素的保护作用,提高紫甘薯花青素的实际应用价值。
为达到上述目的,本发明采用了以下技术方案:
一种紫甘薯花青素微胶囊的制备方法,包括以下步骤:
将含有紫甘薯花青素的芯材分散于囊材溶液中,并在芯材中的紫甘薯花青素分散至囊材溶液的过程中对囊材溶液在20℃~30℃下进行超声处理,得到花青素混合液,所述囊材溶液为β-环糊精水溶液或β-环糊精衍生物水溶液;将花青素混合液在20℃~30℃下避光搅拌均匀后真空冷冻干燥,得到紫甘薯花青素微胶囊。
优选的,所述芯材是通过对紫甘薯中的花青素进行提取以及对所得提取液中的花青素依次经萃取、大孔吸附树脂吸附进行纯化后采用真空冷冻干燥制得的紫甘薯花青素粉体。其中对紫甘薯中花青素的提取采用超声波辅助溶剂法。
优选的,所述超声波辅助溶剂法提取紫甘薯花青素的提取条件包括:干燥(55℃~60℃、12h~24h)后紫甘薯与提取溶剂的比例(料液比)为1:25~1:35,提取时间为40min~60min,提取温度为50℃~60℃,提取溶剂为pH 2~3、体积分数50%~70%的酸化乙醇水溶液或酸化甲醇水溶液。其中,提取溶剂中用于调节该提取溶剂pH的成分(pH调节剂)为HCl、柠檬酸、甲酸或乙酸。
优选的,所述提取液在萃取前依次进行离心、减压浓缩(-0.1MPa~-0.2MPa、40℃~45℃)。
优选的,所述萃取的条件包括:以乙酸乙酯为萃取试剂,萃取2~3次后合并有机相。通过萃取除去黄酮类亲脂性杂质。
优选的,所述吸附的条件包括:吸附柱填料为弱极性聚合物吸附剂(如AB-8大孔吸附树脂),上样pH为2~3,上样量为30~35柱体积(BV),吸附时间为3.5h~4h;解吸液为pH 2~3、体积分数75%~85%的酸化乙醇水溶液或酸化甲醇水溶液,解吸液用量为10~15柱体积(BV),解吸时间为3.5h~4.5h。其中,解吸液中用于调节该解吸液pH的成分(pH调节剂)为HCl、甲酸或乙酸。
优选的,所述吸附柱的洗脱包括以下步骤:先用酸化后的蒸馏水(pH 2.5~3.5,pH调节剂为HCl、甲酸或乙酸)洗脱吸附柱直至洗脱液无色,以除去蛋白质、糖类等水溶性杂质;再用所述解吸液洗脱吸附柱上的紫甘薯花青素。
优选的,所述吸附柱上的紫甘薯花青素经洗脱所得洗脱液在真空冷冻干燥前进行减压浓缩。
优选的,所述β-环糊精衍生物选自羧甲基-β-环糊精或磺丁基-β-环糊精。
优选的,所述囊材溶液的囊材质量分数为1%~5%,溶剂为pH 2.6~3.0的缓冲体系(如醋酸-醋酸钠缓冲体系)。
优选的,所述芯材(如上述紫甘薯花青素粉体)的用量按所述缓冲体系中芯材与囊材的质量比(芯囊比)计为1:3~1:10。
优选的,所述超声处理的时间是按照使芯材(如上述紫甘薯花青素粉体)中的紫甘薯花青素全部溶解而确定,所述花青素混合液的避光搅拌时间为12h~24h、搅拌转速为50r.min-1~70r.min-1,超声处理及避光搅拌的温度条件为20℃~30℃。即通过超声处理和搅拌,使缓冲体系中的囊材和芯材充分作用。
本发明的有益效果体现在:
本发明以天然植物活性物质紫甘薯花青素为包合对象,通过将β-环糊精类囊材和芯材混匀,并经过超声及搅拌使其充分作用后真空冷冻干燥,从而实现对紫甘薯花青素进行微胶囊化包合,不仅解决了紫甘薯花青素在实际应用过程中稳定性低的问题,而且获得了良好的包合效果,为紫甘薯花青素的产业化开发提供了科学、可靠的实践依据。
附图说明
图1为紫甘薯花青素初提液的高效液相色谱分析图;图中:A代表提取阶段的浓缩液;B代表芍药色素-3-[6-(E)-咖啡酰-2-{6-咖啡酰葡萄糖苷}葡萄糖苷]-5-葡萄糖苷对照品;C代表芍药色素-3-[6-(E)-咖啡酰-2-{6-对羟基苯甲酰葡萄糖苷}葡萄糖苷]-5-葡萄糖苷对照品;D代表芍药色素-3-[6-(E)-咖啡酰-2-{6-(E)-阿魏酰葡萄糖苷}-葡萄糖苷]-5-葡萄糖苷对照品。
图2为实施例1制备的以磺丁基-β-环糊精为囊材的紫甘薯花青素微胶囊的不同放大倍率扫描电镜图。
图3为紫甘薯花青素冻干粉的不同放大倍率扫描电镜图。
图4为囊材(Capsule materials)选择对微胶囊的产率(Production yield)及其紫甘薯花青素包埋率(Encapsulation efficiency)影响(*表示组间存在显著性差异)。
图5为不同芯囊比(Core-capsule ratio)对微胶囊的产率及其紫甘薯花青素包埋率的影响(*表示组间存在显著性差异)。
图6为不同囊材质量分数(Capsule material mass fraction)对微胶囊的产率及其紫甘薯花青素包埋率的影响(*表示组间存在显著性差异)。
图7为储存条件对不同浓度药物(紫甘薯花青素微胶囊)抗氧化能力的影响( n=3),其中,(A)保存于自然光照下;(B)保存于黑暗处(a:1μg.mL-1;b:5μg.mL-1;c:10μg.mL-1;d:20μg.mL-1;e:40μg.mL-1;f:60μg.mL-1;g:80μg.mL-1;h:100μg.mL-1)。
图8为储存条件对紫甘薯花青素微胶囊热稳定性和光照稳定性的影响(a-d:紫甘薯花青素微胶囊;e-h:紫甘薯花青素;a、e:25℃2自然光;b、f:25℃2黑暗;c、g:37℃2自然光;d、h:37℃2黑暗)。
具体实施方式
下面结合附图和实施例对本发明作进一步详细描述。所述实施例仅用于解释本发明,而非对本发明保护范围的限制。
实施例1
本实施例利用β-环糊精、不同β-环糊精衍生物分别制备紫甘薯花青素微胶囊,具体过程如下:
(1)紫甘薯花青素的提取:将洗净的鲜紫苷薯切成约3mm的厚片,60℃下干燥12h,经过高速粉碎机粉碎后过80目筛,得紫苷薯原料,4℃冷藏保存。在提取溶剂为60%(v:v)的乙醇溶液(pH=2,HCl)、料液比1:30(g:mL),超声时间60min及超声温度60℃的最佳工艺条件下,采用恒温数控超声波清洗机提取紫甘薯花青素,将提取液在4000r.min-1下离心10min,收集上清液,然后在旋转蒸发仪上进行减压蒸馏(-0.1MPa、40±0.1℃;用锡纸包裹蒸馏瓶以实现避光操作),收集浓缩液。
其中,60%(v:v)的乙醇溶液(pH=2,HCl)的配制:取12mol·L-1的市售浓盐酸用蒸馏水稀释60倍,得0.2mol·L-1的盐酸溶液,然后将上述盐酸溶液和无水乙醇按4:6(v:v)进行混合,采用pH计并以盐酸为调节剂调节混合溶液pH=2。
采用高效液相色谱法对上述浓缩液进行分析,色谱条件如下。
色谱柱:Agilent ZORBAX SB-C18,5μm,4.6×250mm。
流动相:0.4%磷酸水溶液为A相,乙腈为B相。
洗脱方式及程序:梯度洗脱;0~2min,B相8%,2~4min,B相12%,4~7min,B相18%,7~12min,B相20%,12~14min,B相25%,14~17min,B相35%,17~23min,B相20%,23~25min,B相8%,25~27min,B相8%。
柱温:30℃;流速:1mL.min-1;检测波长:524nm。
由图1可知各对照品色谱峰峰形对称,浓缩液样品中对照品成分色谱峰保留时间与各自对照品溶液中的保留时间一致,且分离度符合要求(>1.5),即成功提取到了紫甘薯花青素。
(2)紫甘薯花青素的纯化:在室温(25℃±5℃)下,将1000mL的分液漏斗用锡纸包裹,每次用500mL乙酸乙酯将500mL浓缩液在暗处进行萃取,连续操作三次(第一次分离的水相再次萃取,第二次分离的水相再次萃取,合并三次的有机相,作为萃取液),萃取液以0.45μm的聚偏氟乙烯微孔滤膜进行过滤处理,再用三蒸水稀释至吸光度0.8左右后用HCl调节pH,然后利用装填有AB-8大孔吸附树脂的吸附柱提纯紫甘薯花青素(最佳工艺条件:上样pH=2,上样量=30BV,吸附时间=4h),达到吸附时间后先用酸化后的蒸馏水(pH=3,HCl)洗脱吸附柱直至洗脱液无色,再用13BV 80%(v:v)的乙醇溶液(pH=2,HCl)以洗脱速率为1mL.min-1对吸附柱上的紫甘薯花青素进行洗脱(最佳工艺条件:解吸时间=4h),收集得到的紫甘薯花青素洗脱液。
其中,80%(v:v)的乙醇溶液(pH=2,HCl)的配制:取12mol·L-1的市售浓盐酸用蒸馏水稀释60倍,得0.2mol·L-1的盐酸溶液,然后将上述盐酸溶液和无水乙醇按2:8(v:v)进行混合,采用pH计并以盐酸为调节剂调节混合溶液pH=2。
酸化后的蒸馏水(pH=3,HCl)的配制:取12mol·L-1的市售浓盐酸用蒸馏水稀释120倍,得0.01mol·L-1的稀盐酸溶液,采用pH计并以盐酸为调节剂调节上述稀盐酸溶液pH=3。
(3)紫甘薯花青素芯材的准备:将紫甘薯花青素洗脱液以旋转蒸发仪在避光下进行减压蒸馏(-0.1MPa、40±0.1℃)除去乙醇后置于培养皿中,在-20℃冰箱冷冻24h后,在避光条件下进行真空冷冻干燥72h,得到紫甘薯花青素冻干粉。
(4)不同囊材对紫甘薯花青素的包合:以pH=2.6的醋酸-醋酸钠缓冲体系分别配制浓度2.5%(w:w)的β-环糊精(β-CD)、羧甲基-β-环糊精(CM-β-CD)、磺丁基-β-环糊精(SBE-β-CD)三种β-环糊精类囊材溶液各20mL,对每一种囊材溶液再按芯囊比(芯材与囊材本身的比例)=1:5(w:w)分别加入纯净的紫甘薯花青素(即上述冻干粉),室温下超声10min使其全部溶解,得到花青素混合液(几乎透明的深红色溶液),在室温下避光磁力搅拌花青素混合液24h(转速为60r.min-1),然后置于培养皿中,在-20℃冰箱冷冻24h后,在避光条件下进行真空冷冻干燥72h,制得紫甘薯花青素微胶囊。
如图2、图3所示,紫甘薯花青素微胶囊化前后形态发生明显变化,微胶囊样品表面粗糙且伴有不规则折痕,而花青素呈现不同尺寸的碎片结构,说明花青素与SBE-β-CD之间可以发生了良好的相互作用;结果表明β-环糊精类囊材可以通过包合紫甘薯花青素形成无定形微胶囊。
如图4所示,β-环糊精、不同β-环糊精衍生物对紫甘薯花青素的包埋率为48.0%~99.6%,紫甘薯花青素微胶囊的产率为55.4%~83.7%。其中磺丁基-β-环糊精(囊材质量分数2.5%、芯囊比=1:5)具有最高的包埋率和产率。
经过其他实验,对上述β-环糊精衍生物包埋率显著高于β-CD的原因进行如下解释说明:环糊精独特的分子结构使其具有优异的包合特性,但β-CD在室温下溶解度不高,且易形成分子内氢键,导致其内部空腔减小,无法实现对花青素分子的完全包合,较多的花青素附着β-CD的表面,从而导致微胶囊的包埋率和产率较低。SBE-β-CD和CM-β-CD是通过化学法修饰制备的改性环糊精,其水溶性明显提高,因此避免了疏水空腔的减小。同时,当pH<4时,β-CD为中性,SBE-β-CD以负离子、CM-β-CD(pKa<4)以分子形式存在,而花青素分子以正离子形式存在,因此SBE-β-CD与花青素分子之间除了具有范德华力和氢键作用,还具有较强的静电相互作用。而步骤4中的超声将有助于囊材和芯材充分溶解以有利于二者进一步发生相互作用,而搅拌使二者处于一种动态平衡,以加快其相互作用,在此过程中,转速不宜过快,以使溶液呈旋涡式均匀旋转为宜,在经一定的搅拌时间(推荐18h~24h)后,缓冲溶液体系颜色会变为均匀的暗红色(颜色较超声处理后加深),此时囊材完成了对芯材的包合作用。
实施例2
本实施例利用磺丁基-β-环糊精(SBE-β-CD)制备紫甘薯花青素微胶囊(主要是调整不同的芯囊比),具体过程如下:
采用与实施例1相同的紫甘薯花青素芯材,先以pH=2.6的醋酸-醋酸钠缓冲体系平行配制三份浓度2.5%(w:w)的磺丁基-β-环糊精(SBE-β-CD)溶液20mL作为囊材溶液,再分别按芯囊比=1:3、1:5、1:10(w:w)加入紫甘薯花青素芯材,室温下超声10min使其全部溶解于相应份囊材溶液,得到三份花青素混合液,在室温下避光磁力搅拌各份花青素混合液24h(转速为60r.min-1),然后置于培养皿中,在-20℃冰箱冷冻24h后,在避光条件下进行真空冷冻干燥72h,制得紫甘薯花青素微胶囊。
如图5所示,不同芯囊比下磺丁基-β-环糊精对紫甘薯花青素的包埋率为99.7%~99.8%,紫甘薯花青素微胶囊的产率为72.3%~83.67%。同时,可见芯囊比=1:5时包合效果最佳。
实施例3
本实施例利用磺丁基-β-环糊精(SBE-β-CD)制备紫甘薯花青素微胶囊(主要是调整不同的囊材质量分数),具体过程如下:
采用与实施例1相同的紫甘薯花青素芯材,先以pH=2.6的醋酸-醋酸钠缓冲体系分别配制浓度1%(w:w)、2.5%(w:w)、5%(w:w)的磺丁基-β-环糊精(SBE-β-CD)溶液各20mL作为囊材溶液,再均按芯囊比=1:5(w:w)加入紫甘薯花青素芯材,室温下超声10min使其全部溶解于相应浓度囊材溶液,得到三种花青素混合液,在室温下避光磁力搅拌各花青素混合液24h(转速为60r.min-1),然后置于培养皿中,在-20℃冰箱冷冻24h后,在避光条件下进行真空冷冻干燥72h,制得紫甘薯花青素微胶囊。
如图6所示,不同囊材质量分数下磺丁基-β-环糊精对紫甘薯花青素的包埋率为99.1%~99.3%,紫甘薯花青素微胶囊的产率为81.7%~91.9%。同时,可见囊材质量分数2.5%、5%时包合效果相当。
另取利用磺丁基-β-环糊精(囊材质量分数2.5%、芯囊比=1:5)制备的紫甘薯花青素微胶囊,对其稳定性和活性(DPPH·清除能力)进行了如下考察。
以DPPH·清除率(Clearance rate)为指标考察不同浓度的紫甘薯花青素微胶囊在储存过程中抗氧化活性的变化,由图7(A)可知,所制备的微胶囊在浓度为1μg·mL-1、5μg·mL-1、10μg·mL-1、20μg·mL-1、40μg·mL-1时,DPPH·清除率分别为(10.8±3.9)%、(23.3±1.0)%、(39.0±0.6)%、(66.8±0.5)%、(94.8±0.3)%,在25℃、自然光下放置100d后,清除率分别降低至(2.3±0.1)%、(11.6±0.3)%、(24.1±0.4)%、(46.0±0.3)%、(79.0±0.1)%;由图7(B)可知,微胶囊在25℃、黑暗处放置100d后,清除率分别降低至(1.9±0.1)%、(11.3±0.3)%、(24.9±0.4)%、(46.1±0.6)%、(80.1±0.3)%,与自然光照条件下相比,DPPH·清除率未发生明显变化。以上结果表明,由SBE-β-CD对紫甘薯花青素进行微胶囊化,可明显改善紫甘薯花青素的光稳定性。
参见图8,在25℃、黑暗条件下,紫甘薯花青素微胶囊和紫甘薯花青素样品在90d的保存率(Preservation rate)分别降低至(82.1±1.1)%和(55.2±1.3)%,在25℃、自然光照下两种样品的保存率分别降低至(80.5±0.3)%和(52.6±0.4)%,这表明储存时间的增加会降低紫甘薯花青素微胶囊和紫甘薯花青素样品的保存率,但紫甘薯花青素微胶囊样品的保存率均明显优于紫甘薯花青素样品,说明微胶囊化提高了紫甘薯花青素的储存稳定性。另外,在37℃、黑暗下放置90d的紫甘薯花青素微胶囊和紫甘薯花青素样品的保存率分别降至(82.1±1.5)%和(38.1±0.7)%,37℃、自然光下两种样品的保存率分别降至(77.8±0.6)%和(34.3±0.3)%,可以看出光线会对两种样品产生不同程度的影响,使其中富含的花青素发生降解反应,同时温度和光照的协同作用会使花青素降解得更快,但紫甘薯花青素微胶囊样品的保存率均显著高于紫甘薯花青素样品,且与25℃下的保存率相差不大,这表明微胶囊化也明显提高了紫甘薯花青素的热稳定性。以上结果表明,由SBE-β-CD对紫甘薯花青素进行微胶囊化,可以对紫甘薯花青素实现良好的包合效果,使其在储存过程中对光线和温度的敏感性降低,提高紫甘薯花青素的稳定性。
本发明具有以下特点:
1、本发明选择紫甘薯为原料提取花青素,克服了目前工业生产中以蓝莓、红葡萄等为原料所引发的资源不足、成本高等问题,具有较大的实际生产应用价值。
2、本发明选择β-环糊精、β-环糊精衍生物作为囊材,种类多、选择范围大,并且不影响芯材的抗氧化活性、与芯材具有良好的生物相容性,同时提供了提高包合效果的途径(如采用磺丁基-β-环糊精可以提高紫甘薯花青素微胶囊的包埋率及产率及紫甘薯花青素稳定性)。
3、本发明基于真空冷冻干燥法制备紫甘薯花青素微胶囊,工艺路线(超声-搅拌-冻干)简单,不但提高了紫甘薯花青素的稳定性,便于紫甘薯花青素的运输、储存和使用,而且对β-环糊精类囊材的包合效果发挥协同增效作用。
Claims (10)
1.一种紫甘薯花青素微胶囊的制备方法,其特征在于:包括以下步骤:
将含有紫甘薯花青素的芯材分散于囊材溶液中,并在芯材中的紫甘薯花青素分散至囊材溶液的过程中对囊材溶液进行超声处理,得到花青素混合液,所述囊材溶液为β-环糊精溶液或β-环糊精衍生物溶液;将花青素混合液避光搅拌均匀后真空冷冻干燥,得到紫甘薯花青素微胶囊。
2.根据权利要求1所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述芯材是通过对紫甘薯中的花青素进行提取以及对所得提取液中的花青素依次经萃取、大孔吸附树脂吸附进行纯化后采用真空冷冻干燥制得的紫甘薯花青素粉体。
3.根据权利要求2所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述紫甘薯中花青素的提取采用超声波辅助溶剂法,提取条件包括:干燥后紫甘薯与提取溶剂的料液比为1:25~1:35,提取时间为40min~60min,提取温度为50℃~60℃,提取溶剂为pH 2~3、体积分数50%~70%的酸化乙醇溶液或酸化甲醇溶液。
4.根据权利要求2所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述提取液在萃取前依次进行离心、减压浓缩;所述萃取的条件包括:以乙酸乙酯为萃取试剂,萃取2~3次后合并有机相。
5.根据权利要求2所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述吸附的条件包括:吸附柱填料为弱极性聚合物吸附剂,上样pH为2~3,上样量为30~35柱体积,吸附时间为3.5h~4h;解吸液为pH 2~3、体积分数75%~85%的酸化乙醇溶液或酸化甲醇溶液,解吸液用量为10~15柱体积,解吸时间为3.5h~4.5h。
6.根据权利要求5所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述吸附柱的洗脱包括以下步骤:先用pH 2.5~3.5的酸化水洗脱吸附柱直至洗脱液无色,再用所述解吸液洗脱吸附柱上的紫甘薯花青素;所述吸附柱上的紫甘薯花青素经洗脱所得洗脱液在真空冷冻干燥前进行减压浓缩。
7.根据权利要求1所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述β-环糊精衍生物选自羧甲基-β-环糊精或磺丁基-β-环糊精。
8.根据权利要求1所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述囊材溶液的质量分数为1%~5%,溶剂为pH 2.6~3.0的缓冲体系。
9.根据权利要求1所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述芯材的用量按芯材与囊材的质量比计为1:3~1:10。
10.根据权利要求1所述一种紫甘薯花青素微胶囊的制备方法,其特征在于:所述超声处理的时间是按照使芯材中的紫甘薯花青素全部溶解而确定,所述花青素混合液的避光搅拌时间为12h~24h、搅拌转速为50r.min-1~70r.min-1,超声处理及避光搅拌的温度条件为20℃~30℃。
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