CN116769190A - 一种烟用环糊精基香料乳液凝胶的制备方法 - Google Patents
一种烟用环糊精基香料乳液凝胶的制备方法 Download PDFInfo
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Abstract
本发明涉及一种烟用环糊精基香料乳液凝胶的制备方法：将改性环糊精加入烟用香料、水中，通过均质乳化制备高油相水包油型Pickering乳液，再将此乳液加入到改性聚乙烯醇中，制备获得。本发明是将环糊精进行琥珀酰化增加其乳化性能，利用改性环糊精乳化包裹烟用香精料，然后加入到丁二酸改性的聚乙烯醇胶中，制备载有烟用香精料纳米油滴的乳液凝胶。该烟用环糊精基香料乳液凝胶可涂布应用于卷烟纸、再造烟草薄片或应用于卷烟搭扣胶，赋予卷烟特定的香气，同时具有持久的贮存稳定性。
Description
技术领域
本发明属于乳液凝胶技术领域，具体涉及一种烟用环糊精基香料乳液凝胶、制备方法及其应用。
背景技术
在卷烟生产过程中，希望通过添加烟用风味成分或香料来提高卷烟的香气及风味，降低杂味或刺激性不良味道，但这些烟用风味或香味中很多重要风味成分都是不溶于水且易挥发的小分子成分，在烟用风味浸膏的制备过程中及卷烟制作过程中很容易导致大量易挥发风味成分的损失，严重影响卷烟的增香效果以及后期贮存中的品质稳定性。如何解决这些重要的风味成分在卷烟中的稳定添加及减少贮存期的挥发损失，是烟草工业面临的一个重要挑战。
针对以上问题，将挥发性香料包裹起来加以应用是一个很好的途径，由此开发出烟用香料的各类微胶囊产品。比如，采用高分子壁材和香精料芯材混合后进行喷雾干燥，这种微胶囊制备方法比较简单但相对粗放，包埋率不高。在目前较为流行的一种加香方式是爆珠，即用高分子聚合物包裹烟用香精料制成密封的脆质胶囊，然后添加至卷烟滤嘴中，抽吸时通过压迫爆珠使香料即时释放、实现增香保润等目的。爆珠卷烟由于将香精料包裹密封成爆珠，防止了挥发性香味成分的贮存损失，因此具有理想的保香增香效果。但爆珠加工质量控制要求高，爆珠易受环境温湿度影响而出现变形或破损，爆珠破碎后短时间内香料主要分布于破碎爆珠所处的局部区域，迁移率较低。近来也有研究将香精料制成乳液凝胶后添加进卷烟，这是一种具有前景的卷烟增香方式，但增香效果与乳液类型及其释放特性有很大关系。
基于此，研发了本申请。
发明内容
本发明目的在于克服现有技术缺陷，提供一种烟用环糊精基香料乳液凝胶，其将改性环糊精稳定的香精料Pickering乳液添加进改性聚乙烯醇中制备成烟用增香凝胶，不仅具有稳定持久的增香特性，而且应用方式简单易行。
本发明还提供了一种上述烟用环糊精基香料乳液凝胶的制备方法及其应用。
为实现上述目的，本发明采用如下技术方案：
一种烟用环糊精基香料乳液凝胶的制备方法，其包括如下步骤：
1）配制环糊精水溶液，搅拌下滴加辛烯基琥珀酸酐的乙醇混合体系（即，将辛烯基琥珀酸酐用1-5倍体积的乙醇稀释获得），滴加过程中控制体系pH 维持在 8.5-9.0之间，滴加完毕，待体系pH不再降低说明反应完成，然后用HCl 溶液中和以调节pH至6.5-7.0，冷冻干燥，经洗涤、真空干燥、粉碎过筛，获得改性环糊精（也称作“辛烯基琥珀酰环糊精乳化稳定剂”）；
滴加过程中，可以将pH计电极插入反应液以监测反应体系的pH值。随着反应的进行体系pH会逐渐降低，需及时滴加3%NaOH溶液使反应体系 pH 维持在 8.5 ~ 9.0之间。待所需辛烯基琥珀酸酐量全部滴加完毕，反应体系pH不再降低表示反应完成；
2）称取改性环糊精，加入香料、水，然后进行高压均质或高速均质处理，获得改性环糊精包合物纳米颗粒稳定的水包油型 Pickering 乳液；
3）配制聚乙烯醇水溶液，加入丁二酸，然后于40-80℃保温0.5-3小时进行改性反应，获得改性聚乙烯醇；
4）将步骤2）制备所得水包油型 Pickering 乳液与步骤3）制备所得改性聚乙烯醇低速混合均匀，即得可通过涂布施用的烟用环糊精基香料乳液凝胶。
本发明制备方法中，以辛烯基琥珀酰环糊精为乳化稳定剂，通过高速或高压均质制备高油相Pickering乳液，乳液中油滴直径在1um以下；以丁二酸交联改性的聚乙烯醇为外相添加剂，以提升乳液的稳定性、施布性。
具体的，步骤1）中，所述环糊精水溶液的质量百分比浓度为5-20%，所述辛烯基琥珀酸酐的添加量不超过环糊精质量的20%。环糊精取代度为DS0-0.15。
上述的制备方法中，具体的，步骤2）中，香料、水的混合体系中，香料体积百分比在60%以上；改性环糊精与香料水混合体系可以按料液比2-20g：100ml进行添加。Pickering乳液中，油相比例优选为40-80%。
本发明所用香料可为非极性的天然提取的烟草风味成分或其他天然提取的植物风味成分，也可以是非极性的人工合成的烟用香精香料成分。进一步的，所述香料可以为薄荷醇、柠檬醛、迷迭香、肉桂醛、香橙精油等中的一种或多种。
进一步的，步骤2）中，可以采用高压均质机在压力10-30 MPa下进行高压均质，可循环处理2-4次，或者也可以在转速10000r/min以上进行高速均质；均质时间为1-5min。
具体的，步骤3）中，配制3-10 wt%（质量百分比）的聚乙烯醇水溶液，聚乙烯醇与丁二酸的质量比优选为10：1-3。
具体的，步骤4）中，水包油型 Pickering 乳液与改性聚乙烯醇的添加比例为5-15ml：100g。
本发明提供了采用上述制备方法制备所得的烟用环糊精基香料乳液凝胶。
本发明还提供了上述烟用环糊精基香料乳液凝胶在再造烟草薄片、卷烟纸或卷烟搭扣胶中的涂布应用。
环糊精是由6-8 个葡萄糖组成的环状低聚糖，圆锥形分子具有一个疏水空腔和亲水外表面，可包埋油相分子形成分子包合物。将环糊精进行辛烯基琥珀酰化后乳化能力进一步增强，辛烯基琥珀酰环糊精包合物的纳米颗粒能够乳化水油体系形成水包油型Pickering 乳液。Pickering乳液不仅可容纳高比例油相，而且油滴直径可控制在数十纳米，稳定性好，是制备油相微胶囊的优秀模板。但Pickering乳液属于结构类乳液，在稀释及干燥过程中易于破乳，通过调整外水相粘稠度可有效解决这一缺陷。聚乙烯醇或改性聚乙烯醇是卷烟制作过程中常用的一类凝胶类添加剂，聚乙烯醇具有良好的粘稠度及附着力，可涂布应用于卷烟材料。本发明将改性环糊精稳定的香精料Pickering乳液添加进改性聚乙烯醇中制备烟用增香凝胶，不仅具有稳定持久的增香特性，而且应用方式简单易行。
本发明中，首先对环糊精进行辛烯基琥珀酸酐湿法处理制备辛烯基琥珀酰环糊精，增强乳化能力；然后利用高压或高速均质法制备改性环糊精包合物纳米颗粒稳定的水包油型 Pickering 乳液，所用香精料为各类常用烟用香精油；再利用丁二酸对聚乙烯醇进行湿热改性，增加其附着力及抗水性，最后将所得Pickering乳液加入改性聚乙烯醇中均匀混合，即得可通过涂布施用的环糊精基香料乳液凝胶。
本发明是将环糊精进行琥珀酰化增加其乳化性能，利用改性环糊精乳化包裹烟用香精料，然后加入到丁二酸改性的聚乙烯醇胶中，制备载有烟用香精料纳米油滴的乳液凝胶。和现有技术相比，本发明的有益效果如下：
1）通过改性环糊精稳定的高油相乳液将烟用香精料完全包裹起来，防止制备及贮存期间香精料的不稳定及挥发损失；
2）利用改性聚乙烯醇的胶黏性及涂布附着性，赋予香精料乳液的稳定性及应用特性；
3）该烟用香味凝胶可以应用于卷烟烟叶、再造烟叶中，在香烟贮存期香气不会挥发损失；在卷烟吸食过程中，通过高温受热作用下风味香料成分释出，赋予卷烟特有香气质，并柔和烟气，改善吸食品质；
4）对卷烟产品而言，本香料凝胶中所含改性环糊精、改性聚乙烯醇以及香精料均为常用成分，无毒无害；制备方法方便易行、经济适用，且环境友好；
5）该烟用环糊精基香料乳液凝胶可涂布应用于卷烟纸、再造烟草薄片或应用于卷烟搭扣胶，赋予卷烟特定的香气，同时具有持久的贮存稳定性。
具体实施方式
以下结合实施例对本发明的技术方案作进一步地详细介绍，但本发明的保护范围并不局限于此。
下述实施例中，如无特殊说明，所用原料均为可以直接购买到的普通市售产品或者可以采用本领域常规技术制备获得。
实施例1
一种烟用环糊精基香料乳液凝胶的制备方法，其包括如下步骤：
（1）准确称量10g β-环糊精分散在100mL去离子水中，60℃加热搅拌使环糊精溶解，获得约9%的环糊精水溶液。称取相当于环糊精质量5%的辛烯基琥珀酸酐，将其用3倍体积无水乙醇进行稀释，然后逐滴加入到环糊精水溶液中，在滴加及反应过程中滴加3% NaOH溶液以控制反应体系 pH 在 8.5 ~ 9.0之间，滴加完毕，待反应体系pH不再降低，说明反应完成。然后用HCl 溶液回调反应溶液的pH值至6.7。冷冻干燥（采用常规冻干方法。通常先冷冻至-35 ~ -40℃使样品成固态，水冻结为冰，再抽真空至5-20Pa使冰升华，从而除去样品中大部分水分），将冷冻干燥过的改性环糊精用异丙醇洗涤杂质，再真空干燥，粉碎过筛，即得辛烯基琥珀酰环糊精乳化稳定剂，该改性环糊精的取代度为0.0536，得率78.4%；
（2）称取5g上述制备所得改性环糊精，加入35mL去离子水，搅拌均匀后加入薄荷醇65mL，利用高压均质法（循环三次均质：第一次30Mpa，第二次20MPa，第三次15MPa）进行处理，每次1min，获得改性环糊精包合物纳米颗粒稳定的水包油型 Pickering 乳液。所得乳液呈乳白色半固体，平均粒径586nm；
（3）称取5g聚乙烯醇，加入100mL水搅拌溶解。加入0.5g丁二酸，然后于60℃保温1小时进行改性反应，获得改性聚乙烯醇；
（4）取10 mL步骤（2）制备所得水包油型 Pickering乳液，加入到100 g步骤（3）制备所得改性聚乙烯醇中，低速搅拌5小时使其均匀混合，即得可通过涂布施用的烟用环糊精基香料乳液凝胶，凝胶中薄荷醇含量约为6.5mL/100g。
实施例2
一种烟用环糊精基香料乳液凝胶的制备方法，其包括如下步骤：
（1）准确称量5g β-环糊精分散在50mL去离子水中，60℃加热搅拌使环糊精溶解，获得约9%的环糊精水溶液。称取相当于环糊精质量3%的辛烯基琥珀酸酐，将其用3倍无水乙醇进行稀释，然后逐滴加入到环糊精水溶液中，在滴加及反应过程中滴加3% NaOH溶液以控制反应体系 pH 在 8.5 ~ 9.0之间，滴加完毕，待反应体系pH不再降低，说明反应完成。用HCl 溶液回调反应溶液的pH 值至6.7，然后冷冻干燥（同上），将冷冻干燥过的改性环糊精用异丙醇洗涤杂质，再真空干燥，粉碎过筛，即得辛烯基琥珀酰环糊精乳化稳定剂，该改性环糊精的取代度为0.0322，得率85.5%；
（2）称取2.5g上述制备所得改性环糊精，加入15mL去离子水，搅拌均匀后加入薄荷醇35mL，利用高速均质法（11000rpm，2min）进行处理，获得改性环糊精包合物纳米颗粒稳定的水包油型 Pickering 乳液。所得乳液呈乳白色半固体，平均粒径326nm；
（3）称取5g聚乙烯醇，加入100mL水搅拌溶解。加入0.5g丁二酸，然后于60℃保温1小时进行改性反应，获得改性聚乙烯醇；
（4）取6 mL步骤（2）制备所得水包油型 Pickering乳液，加入到100 g步骤（3）所得改性聚乙烯醇中，低速搅拌3小时使均匀混合，即得可通过涂布施用的烟用环糊精基香料乳液凝胶，凝胶中薄荷醇含量约为4.2 mL/100g。
将上述实施例1和2制备所得香料乳液凝胶进行再造烟叶片基的喷布，喷涂工序设置在浓缩液涂布之后，喷涂量为100 mL/m2片基，90℃下烘干，切丝后卷制成烟支，在温度22℃、相对湿度65%环境下平衡48 h后检测评价，以喷涂薄荷精油的丙二醇溶液为对照。评价结果见下表1。
表1 薄荷精油Pickering乳液凝胶添加样品评价
上表1的评价结果显示：与对照样相比，添加薄荷精油乳液凝胶的样品，其薄荷香气释放均匀、稳定，与烟香谐调，抽吸舒适感较好。随着精油凝胶添加量提高，其香气强度也明显上升，香气透发性增加。
评价实施中发现，新卷制实施例1、2对照样烟支薄荷香气浓郁，但经过两周存后放其香气明显转淡，抽吸时薄荷香气不突出。而新制及存放的实施例1、2薄荷精油乳液凝胶烟支具有淡淡薄荷香气，抽吸时薄荷气息突出，清凉舒适。这说明薄荷精油经过本发明Pickering乳液工艺以微胶囊形式存在于再造烟叶丝中，不易挥发损失，提供再造烟叶稳定而清凉舒适的吸食品质。
Claims (9)
1.一种烟用环糊精基香料乳液凝胶的制备方法，其特征在于，包括如下步骤：
1）配制环糊精水溶液，搅拌下滴加辛烯基琥珀酸酐的乙醇混合体系，滴加过程中控制体系pH 维持在 8.5-9.0之间，滴加完毕，待体系pH不再降低说明反应完成，然后调节pH至6.5-7.0，冷冻干燥，经洗涤、真空干燥、粉碎过筛，获得改性环糊精；
2）称取改性环糊精，加入香料、水，然后进行高压均质或高速均质处理，获得改性环糊精包合物纳米颗粒稳定的水包油型 Pickering 乳液；
3）配制聚乙烯醇水溶液，加入丁二酸，然后于40-80℃保温0.5-3小时进行改性反应，获得改性聚乙烯醇；
4）将步骤2）制备所得水包油型 Pickering 乳液与步骤3）制备所得改性聚乙烯醇混合均匀，即得。
2.如权利要求1所述烟用环糊精基香料乳液凝胶的制备方法，其特征在于，步骤1）中，所述环糊精水溶液的质量百分比浓度为5-20%，所述辛烯基琥珀酸酐的添加量不超过环糊精质量的20%。
3.如权利要求1所述烟用环糊精基香料乳液凝胶的制备方法，其特征在于，步骤2）中，香料、水的混合体系中，香料体积百分比在60%以上；改性环糊精与香料水混合体系按料液比2-20g：100ml进行添加。
4.如权利要求3所述烟用环糊精基香料乳液凝胶的制备方法，其特征在于，所述香料为薄荷醇、柠檬醛、迷迭香、肉桂醛、香橙精油中的一种或多种。
5.如权利要求3所述烟用环糊精基香料乳液凝胶的制备方法，其特征在于，采用高压均质机在压力10-30 MPa下进行高压均质，或者在转速10000r/min以上进行高速均质；均质时间为1-5min。
6.如权利要求1所述烟用环糊精基香料乳液凝胶的制备方法，其特征在于，步骤3）中，配制3-10 wt%的聚乙烯醇水溶液，聚乙烯醇与丁二酸的质量比为10：1-3。
7.如权利要求1所述烟用环糊精基香料乳液凝胶的制备方法，其特征在于，步骤4）中，水包油型 Pickering 乳液与改性聚乙烯醇的添加比例为5-15mL：100g。
8.采用权利要求1至7任一所述制备方法制备所得的烟用环糊精基香料乳液凝胶。
9.权利要求8所述烟用环糊精基香料乳液凝胶在再造烟草薄片、卷烟纸或卷烟搭扣胶中的涂布应用。
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