CN112931833A - 一种花椒提取物微胶囊及其制备工艺 - Google Patents
一种花椒提取物微胶囊及其制备工艺 Download PDFInfo
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Abstract
本发明公开了一种花椒提取物微胶囊，包括花椒提取物10~20份，第一保护层50~200份，第二保护层150~600份，第三保护层2~20份，且花椒提取物依次被第一、第二、第三保护层包裹。其中花椒提取物选自花椒精油或花椒油树脂中任意一种。本发明制得的花椒提取物微胶囊的稳定性更强，在氧气、pH值、水分、温度等的破坏下，都能保护花椒提取物的麻度和香气。将本发明制得的花椒提取物微胶囊用于复合调味料中，能有效保持花椒的风味，同时在煮制过程中，能耐100度超过30分钟，延缓香气与麻味物质的释放。
Description
技术领域
本发明属于生物领域，具体为包埋技术领域。涉及一种花椒提取物微胶囊及其制备工艺以及采用该制备工艺制得的花椒提取物微胶囊。
背景技术
目前花椒提取物化学成分的研究主要是针对挥发油、酰胺类以及生物碱这三类成分，其中挥发油和酰胺类这两类呈味成分分别反映花椒的香气和麻味特征，而在食品行业中使用花椒，主要取其香麻味，因此这也是花椒品质评价中最为重要的两个特征性指标。此外，花椒中还有一些其他生理活性成分如木脂素、香豆素、脂肪酸、黄酮苷、三萜。和甾醇等。
花椒麻素即花椒油树脂，主要是链状不饱和酰胺，含有大量的共轭三烯键，极易被氧化，花椒提取物因其含有花椒麻素类物质，贮存过程中会缓慢氧化，主要是脂类直接与氧气反应即自动氧化，在这一反应中绝大多数是自由基锁链反应，常会有过氧化物、氢过氧化物、过氧酸的生成，各种过氧化物的形成导致过氧化值的升高。这些中间产物不稳定继续反应最终生成有酸败特征的醛、酮、醇、碳氢化合物等，另外在自动氧化过程中光、酶、金属离子可以催化氧化过程，加速氧化，在货架期内若过氧化值增长较快，风味损失较大。花椒精油的香气组分中有部分易挥发成分，在储存和使用过程中，随着环境温度的增加，易挥发组分失去而容易造成香气的不完整和缺失。
花椒提取物微胶囊化能有效保护花椒化学成分，提供稳定性，减少外界环境（如氧气、pH值、水分、温度等）的破坏，特别是氧化破坏作用；控制或延长芯材的释放速度；隔离组分，使食品体系多样化而不发生相互干扰是现阶段行业内必须克服的困难。既往发明CN109907125A公开了一种稳定性提高的花椒油树脂微胶囊及其制备方法，该专利通过花椒油树脂后高速均质搅拌形成O/W型乳状液，经喷雾干燥后获得花椒油树脂微胶囊粉末，虽然该微胶囊粉末在一定程度上提高了花椒提取物的稳定性，减少外界环境（如氧气、pH值、水分、温度等）的破坏，但是在加工过程中花椒油树脂需要在喷雾干燥过程中承受180℃的高温，造成花椒提取物易挥发性成分的缺失，进而影响香气。同时，这种微胶囊壁材极易溶于水，煮制过程中，造成花椒油树脂很快就溶于水中，花椒油树脂释放速度较快，不利于其延缓释放。
基于此，一种应用于复合调味料中的高花椒提取物，且具备稳定性强、在烹制过程中，不仅能耐高温，同时香味物质与麻味物质能缓慢释放的花椒提取物微胶囊及其制备工艺是行业内急需的。
发明内容
鉴于上述分析，本发明的目的是提供一种花椒提取物微胶囊，进一步提高花椒提取物的稳定性，用于复合调味料中，保持花椒风味，同时在煮制过程中，能耐高温，延缓释放。本发明是通过如下工艺实现的：
一种花椒提取物微胶囊，包括：
花椒提取物；
第一保护层；
第二保护层；以及
第三保护层；
所述花椒提取物依次被第一第一、第二、第三保护层包裹；
所述微胶囊粒径为0.5~5mm。
进一步的，所述花椒提取物为10~20份，第一保护层为50~200份，第二保护层为150~600份，第三保护层为2~20份。
进一步的，所述花椒提取物选自花椒精油或花椒油树脂；
其中花椒精油为重庆华萃生物科技有限公司提供的花椒精油180，批号20200903。
花椒树脂油为陇南利和萃取科技有限公司提供的花椒油树脂LH2202，批号20210114。
进一步的，所述第一保护层选自多孔糊精或变性淀粉作为介质，优选为多孔糊精。
进一步的，所述第二保护层选自棕榈油或起酥油作为介质，优选为棕榈油。
进一步的，所述第三保护层由水凝胶介质与钙离子发生交联反应形成；所述水凝胶介质选自海藻酸钠、果胶、结冷胶、明胶中任意一种。
一种制备花椒提取物微胶囊的工艺，包括：
（1）被第一保护层包裹的花椒提取物的制备：
将第一保护层分散在水中形成过饱和溶液，保持常温持续搅拌，等量乙醇溶解花椒提取物后，匀速滴入过饱和溶液中并持续搅拌约4小时，静置隔夜，花椒提取物经过充分吸附，过滤后用清水洗涤3次，即可得到被第一保护层包裹的花椒提取物，按照重量计算，花椒提取物为10~20份，第一保护层为50~200份；
（2）第二保护层的制备：
将第二保护层在60℃熔化成液体，将步骤（1）所得到的被第一保护层包裹的花椒提取物均匀分散在其中，并持续搅拌，保持温度恒定在60℃，即可得到第二保护层产物，按照重量计算，第二保护层为150~600份；
（3）第三保护层的制备：
将第三保护层配制成重量为1-2%的水溶液，冷水浴是重量为5%的乳酸钙水溶液，利用同心轴管设备，直径为0.3~3mm内层流动第二保护层产物，直径为1~5mm外层流动第三保护层，同时流出，第三保护层将第二保护层包裹住，滴入冷水浴中，第三保护层迅速固化，即可形成第三保护层产物，按照重量计算，第三保护层为2~20份；
（4）成型：
将步骤（3）得到的第三保护层产物常温通风干燥，即可得到一种花椒提取物微胶囊。
本发明还公开了一种上述任一制备工艺制得的花椒提取物微胶囊。
本发明还公开了一种上述任一所述花椒提取物微胶囊在食品加香技术中的应用。
本发明的有益效果在于：
1、本发明制得的花椒提取物微胶囊的稳定性更强，在氧气、pH值、水分、温度等的破坏下，都能保护花椒提取物的麻度和香气。
2、本发明制得的花椒提取物微胶囊用于复合调味料中，能有效保持花椒的风味，同时在煮制过程中，能耐100度超过30分钟，延缓香气与麻味物质的释放。
附图说明
图1为本发明花椒提取物微胶囊的结构示意图。
图2为本发明同心轴管的结构示意图。
具体实施方式
实施例1
一种制备花椒提取物微胶囊的工艺，包括：
（1）被第一保护层包裹的花椒提取物的制备：
将多孔糊精最为介质，分散在水中形成过饱和溶液，保持常温持续搅拌，等量乙醇溶解花椒精油后，匀速滴入过饱和溶液中并持续搅拌约4小时，静置隔夜，花椒提取物经过充分吸附，过滤后用清水洗涤3次，即可得到被第一保护层包裹的花椒提取物，按照重量计算，花椒精油为15份，第一保护层为125份；
（2）第二保护层的制备：
将棕榈油作为介质，在60℃熔化成液体，将步骤（1）得到被第一保护层包裹的花椒提取物均匀分散在其中，并持续搅拌，保持温度恒定在60℃，即可得到第二保护层产物，按照重量计算，第二保护层为375份；
（3）第三保护层的制备：
将海藻酸钠作为介质，配制成重量为1.5%的水溶液，冷水浴是重量为5%的乳酸钙水溶液，利用同心轴管设备，直径为2mm内层流动第二保护层产物，直径为3mm外层流动第三保护层，同时流出，第三保护层将第二保护层包裹住，滴入冷水浴中，第三保护层迅速固化，即可形成第三保护层产物，按照重量计算，第三保护层为10份；
（4）成型：
将步骤（3）得到的第三保护层产物常温通风干燥，即可得到一种花椒提取物微胶囊，微胶囊粒径为3mm。
实施例2
一种制备花椒提取物微胶囊的工艺，包括：
（1）被第一保护层包裹的花椒提取物的制备：
将变性淀粉作为介质，分散在水中形成过饱和溶液，保持常温持续搅拌，等量乙醇溶解花椒油树脂后，匀速滴入过饱和溶液中并持续搅拌约4小时，静置隔夜，花椒提取物经过充分吸附，过滤后用清水洗涤3次，即可得到被第一保护层包裹的花椒提取物，按照重量计算，花椒提取物为10份，第一保护层为50份；
（2）第二保护层的制备：
将起酥油作为介质，在60℃熔化成液体，将步骤（1）所得到被第一保护层包裹的花椒提取物均匀分散在其中，并持续搅拌，保持温度恒定在60℃，即可得到第二保护层产物，按照重量计算，第二保护层为150份；
（3）第三保护层的制备：
将结冷胶作为介质，配制成重量为1%的水溶液，冷水浴是重量为5%的乳酸钙水溶液，利用同心轴管设备，直径为0.3mm内层流动第二保护层产物，直径为1mm外层流动第三保护层，同时流出，第三保护层将第二保护层包裹住，滴入冷水浴中，第三保护层迅速固化，即可形成第三保护层产物，按照重量计算，第三保护层为2份；
（4）成型：
将步骤（3）得到的第三保护层产物常温通风干燥，即可得到一种花椒提取物微胶囊，微胶囊粒径为4mm。
实施例3
一种制备花椒提取物微胶囊的工艺，包括：
（1）被第一保护层包裹的花椒提取物的制备：
将多孔糊精作为介质，分散在水中形成过饱和溶液，保持常温持续搅拌，等量乙醇溶解花椒精油，匀速滴入过饱和溶液中并持续搅拌约4小时，静置隔夜，花椒提取物经过充分吸附，过滤后用清水洗涤3次，即可得到被第一保护层包裹的花椒提取物，按照重量计算，花椒提取物为20份，第一保护层为200份；
（2）第二保护层的制备：
将起酥油作为介质，在60℃熔化成液体，将步骤（1）所得到被第一保护层包裹的花椒提取物均匀分散在其中，并持续搅拌，保持温度恒定在60℃，即可得到第二保护层产物，按照重量计算，第二保护层为600份；
（3）第三保护层的制备：
将果胶作为介质，配制成重量为2%的水溶液，冷水浴是重量为5%的乳酸钙水溶液，利用同心轴管设备，直径为3mm内层流动第二保护层产物，直径为5mm外层流动第三保护层，同时流出，第三保护层将第二保护层包裹住，滴入冷水浴中，第三保护层迅速固化，即可形成第三保护层产物，按照重量计算，第三保护层为20份；
（4）成型：
将步骤（3）得到的第三保护层产物常温通风干燥，即可得到一种花椒提取物微胶囊，微胶囊粒径为5mm。
对比例1
参照申请号CN201910083905.2中公开的技术工艺制得，具体如下：
（1）将超净工作台里面的20W紫外线灯管打开预热20min，使光波稳定在253.7nm。将玉米蛋白粉平铺在直径为9cm的玻璃培养皿中，然后放置于垂直距离紫外线灯下20cm处辐照30min。
（2）称取以上处理过的玉米蛋白粉15.0g，加入250mL蒸馏水，磁力搅拌器搅拌1h，配置成6.0%（w/v）的悬浊液。在500w的超声功率下处理30min后，4000r/min离心10min去除不溶物，制备得到2.0%（w/v）的玉米蛋白粉溶液。
（3）将以上玉米蛋白粉溶液与壳寡糖按质量比1:2混合均匀，溶解分散于250mL蒸馏水，磁力搅拌器搅拌12h，使其混合均匀。调节混合溶液pH至8.0，于80℃水浴加热2h。
（3）再调节上述玉米蛋白和壳寡糖水浴加热反应后反应物的pH至3.0，然后加入250mL***胶溶液，使混合液中壳寡糖与***胶的质量比为2:8，固形物浓度为0.96%（w/v），于80℃水浴继续加热10h后冷却到室温。
（4）再在上述反应液中加入0.2g葡萄酒皮渣多糖（质量百分比占总壁材的4.0%），搅拌混合均匀，混合物中总壁材浓度达到1.0%（w/v）。以此混合物为壁材，加入5.0g花椒油树脂，保持芯壁质量比为1:1，30℃、10000r/min乳化10min，形成O/W型乳状液。
（5）在进风温度为180℃、出风温度为80℃、进样速度为9mL/min的条件下，将所述O/W型乳状液喷雾干燥获得花椒油树脂微胶囊粉末。
本实施例此条件下制备的花椒油树脂微胶囊包埋率为64.5%，花椒油素含量为6.5%；65℃下的油脂加速氧化实验21天时过氧化值为16.9mmol/kg，而未包埋的花椒油树脂的过氧化值为42.6mmol/kg。
对比例2
购买的花椒精油，其中花椒精油为重庆华萃生物科技有限公司提供的花椒精油180，批号20200903。
对比例3
购买的花椒油树脂，花椒树脂油为陇南利和萃取科技有限公司提供的花椒油树脂LH2202，批号20210114。
试验例1
各组样品的麻味物质在不同时间点的检测情况
分别取单位质量的各组实施例与对比例的样品，提取样品的麻味物质，以羟基-α-山椒素作为标准品，配制不同浓度的标准品，绘制标准曲线，用高效液相色谱法进行检测，确定单位质量的各组实施例与对比例的样品的羟基-α-山椒素含量。
测定各组实施例与对比例的样品放入pH=7的清水中经100℃加热60min时各个时间节点分别取样，以上述步骤所得的，单位质量的各组实施例与对比例的样品的羟基-α-山椒素含量数据为基准，检测水中各组样品溶出羟基-α-山椒素含量的变化情况，进而检测麻味成分的变化情况，具体如表1所示。
表1 各组麻味物质在不同时间点的检测情况
根据表1数据显示：实施例1、实施例2、实施例3样品经过100℃加热，球形微胶囊还未完全破裂，可以实现在高温情况下的缓慢释放；对比例1虽然也能实现缓慢释放，但是在15-30分钟时候，缓释体系完全破坏，伴随高温，羟基-α-山椒素持续衰减；对比例2、对比例3由于没有缓释体系的保护，羟基-α-山椒素呈现出高温下持续衰减的现象。
试验例2
测定各组实施例与对比例的样品受环境的影响情况：包括对各组样品进行氧化处理，置于酸性环境与中性环境下进行反应60min。在对各组样品的性能进行测试，具体结果如表2所示。
分别取单位质量的各组实施例与对比例的样品，提取样品的麻味物质，以羟基-α-山椒素作为标准品，配制不同浓度的标准品，绘制标准曲线，用高效液相色谱法进行检测，确定单位质量的各组实施例与对比例的样品的羟基-α-山椒素含量。
测定各组实施例与对比例的样品放入pH=5和pH=7清水中经100℃加热60min时各个时间节点分别取样，以上述步骤所得的，单位质量的各组实施例与对比例的样品的羟基-α-山椒素含量数据为基准，检测水中各组样品溶出羟基-α-山椒素含量的变化情况，进而检测麻味成分的变化情况，具体如表2所示。
表2 各组麻味物质在不同pH环境下时不同时间点的检测情况
根据表2数据显示：实施例1、实施例2在酸性条件下缓释效果优于中性环境，微胶囊呈现出一定的耐酸性；实施例3、在酸性和中性环境下，微胶囊素缓释效果相差不大；对比例2、对比例3对环境的酸性和中性环境敏感性不强，羟基-α-山椒素溶出现象无明显变化；对比例1在酸性条件下，乳化体系遭到破坏，呈现出微胶囊缓释性能变差，不耐酸性环境的现象。
最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，但本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种花椒提取物微胶囊，包括：
花椒提取物；
第一保护层；
第二保护层；以及
第三保护层；
所述花椒提取物依次被第一第一、第二、第三保护层包裹；
所述微胶囊粒径为0.5~5mm。
2.根据权利要求1所述的微胶囊，其中：
所述花椒提取物为10~20份，第一保护层为50~200份，第二保护层为150~600份，第三保护层为2~20份。
3.根据权利要求1或2所述的微胶囊，其中：
所述花椒提取物选自花椒精油或花椒油树脂。
4.根据权利要求1或2所述的微胶囊，其中：
所述第一保护层选自多孔糊精或变性淀粉作为介质。
5.根据权利要求1或2所述的微胶囊，其中：
所述第二保护层选自棕榈油或起酥油作为介质。
6.根据权利要求1或2所述的微胶囊，其中：
所述第三保护层由水凝胶介质与钙离子发生交联反应形成；
所述水凝胶介质选自海藻酸钠、果胶、结冷胶、明胶中任意一种。
7.一种制备权利要求1~6所述任一花椒提取物微胶囊的工艺，包括：
（1）被第一保护层包裹的花椒提取物的制备：
第一保护层分散在水中形成过饱和溶液，保持常温持续搅拌，等量乙醇溶解花椒提取物后，匀速滴入过饱和溶液中充分吸附，过滤洗涤，得到被第一保护层包裹的花椒提取物；
（2）第二保护层的制备：
第二保护层在60℃熔化成液体，将步骤（1）所得被第一保护层包裹的花椒提取物均匀分散在其中，得到第二保护层产物；
（3）第三保护层的制备：
利用同心轴管设备，内层流动第二保护层，外层流动第三保护层，内层与外层同时流出，第三保护层迅速固化，形成第三保护层产物；
（4）成型：
将步骤（3）得到的第三保护层产物常温通风干燥，即可得到一种花椒提取物微胶囊。
8.根据权利要求7所述的制备工艺，其中：
所述同心轴管包括内管和外管，内管直径为0.3~3mm，外管直径为1~5mm。
9.一种根据权利要求7~8所述任一制备工艺制得的花椒提取物微胶囊。
10.一种根据权利要求1~6、或9任一所述的花椒提取物微胶囊在食品加香技术中的应用。
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