CN114073920A - 油性成分微胶囊制备方法 - Google Patents
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Abstract
一种油性成分微胶囊制备方法,包含将水、酪蛋白钠、麦芽糊精与水相乳化剂均匀混合为连续相;将油性成分与油相乳化剂均匀混合为分散相;施加气体压力使所述分散相通过孔隙约1.9μm的多孔玻璃膜(Porous Glass membrane)进入所述连续相,形成粒径均一的乳化液;喷雾干燥所述乳化液制备出具有高承载率、好的缓释性及储藏稳定性的油性成分微胶囊,适合应用于精油等风味物质或鱼油的微胶囊化。
Description
技术领域
本发明是关于一种利用薄膜乳化技术搭配喷雾干燥技术来制备以油性风味物质或机能性成分为芯材的微胶囊。
背景技术
微胶囊化技术是一种可以通过壁材的包覆,提供芯材与外界环境间的物理屏障,进而抵抗环境中的光、温度、氧气以及酸碱等影响,达到延长机能性成分稳定性、控制释放与味道遮蔽等特性。将分散相(dispersed phase) 的芯材均匀分散于连续相(continuousphase)的壁材中,形成稳定的乳化液是微胶囊化制程的关键步骤。食品业界最常使用高压均质乳化技术,透过高压将流体送到均质阀,过程产生剪切力将分散相均匀分散,而得到性状良好的乳化液。但高压均质乳化过程中能源效率(Energy efficiency)仅2%,设备零件在高压操作下容易耗损,且乳化液温度会在过程中上升,易影响热敏感物质,而限缩芯材使用范围。
薄膜乳化技术原理为分散相受到些微的气体增压下通过孔隙均一的多孔玻璃膜(Porous Glass membrane),并在膜表面形成液滴(droplets),在沿膜表面流动的连续相的冲刷作用下,当液滴的直径达到某一值时,就从膜表面剥离,进入连续相而形成乳化液。相对于其他乳化方式,具有低剪切力、低耗能、粒径均一且制程再现性高等优点。
CN105707290A揭示一种粉末鸡油的制造方法,需先将变性淀粉加热至82℃,加入麦芽糊精后降温至60℃,使壁材完全溶解于水中,以均质机于18MPa条件下进行乳化,将乳化液温度保持于60℃,并以入风温度 168℃进行喷雾干燥。
CN102641245揭示一种装载难溶性药物的壳聚糖-壳聚糖衍生物纳米球产品,将难溶性药物溶解于有机溶剂如液体石蜡及石油醚当中作为内油相(O1),以壳聚糖、乳化剂及水作为水相(W),透过均质乳化法制备O1/W 乳化液,再透过多孔膜形成O1/W/O2型乳化液。将上述多重乳化液先以25℃固化1hr,缓慢加热至50℃,再恒温交联反应10hr,离心去除上清液后,即得微胶囊。
尽管膜乳化可制备性状优良的乳化液,但能否在干燥后形成微胶囊仍有技术缺口,因此目前尚无专利将薄膜乳化应用于风味分子微胶囊制程当中。
发明内容
本发明利用薄膜乳化技术搭配喷雾干燥技术制备以风味物质或机能性成分为芯材的微胶囊。
本发明通过乳化剂及壁材的筛选,来维持乳化液的稳定性,并制造出大小均一、高包覆率的微胶囊颗粒。
本发明的微胶囊颗粒具有很好的缓释性及储藏稳定性,并达到风味物质或机能性成分延长释放的目的。
本发明的较佳具体实施例包括(但不限于)下列申请专利范围所描述的实施例。
附图说明
图1显示本发明制备的九层塔香精乳化液于常温(实线)及高温80℃处理0.5小时后(虚线),分别以雷射粒径分析仪LS13 320测量其中分散相的粒径的粒径分布结果。
图2显示本发明的九层塔香精微胶囊与对照例在高温加速性试验 (40℃)期间的酸值的检测结果。
图3显示本发明的九层塔香精微胶囊与对照例在高温***性试验 (60℃)期间的酸值的检测结果。
图4显示本发明的九层塔香精微胶囊与对照例在高温加速性试验 (40℃)期间的硫代巴比妥(TBARS)酸值的检测结果。
图5显示本发明的九层塔香精微胶囊与对照例在高温***性试验 (60℃)期间的硫代巴比妥(TBARS)酸值的检测结果。
图6显示本发明的九层塔香精微胶囊与对照例在高温***性试验 (60℃)期间的香精包覆率变化。
图7显示以气相层析质谱仪(GC-MS)检测九层塔香精以及九层塔香精微胶囊的风味分子成分及含量,检测结果显示,风味分子主要为草蒿(Estragole),占所有风味分子90%以上。
图8显示本发明的九层塔香精微胶囊与对照例在高温***性试验 (60℃)期间的草蒿含量变化。
具体实施方式
以下预备例及实施例使用下列的材料及仪器设备。
材料:
九层塔香精(SWEET BASIL FLAVOR MC-20PM)购自广福林有限公司(桃园,台湾地区);
酪蛋白钠(SODIUM CASEINATE)购自模里西斯商台纽股份有限公司台湾分公司(桃园,台湾地区);
麦芽糊精(Maltodextrin)购自环太企业有限公司(桃园,台湾地区);
***胶(Gum Arabic)购自台湾***胶有限公司(台北,台湾地区);
乳化剂:聚山梨醇酯80(Polysorbate 80)或称Tween 80、聚山梨醇酯 60(Tween60)、聚山梨醇酯20(Tween 20)、聚蓖麻油酸聚甘油-3酯 (Polyglyceryl-3-Polyricinoleate)(2253)、单硬脂酸甘油酯(Glyceryl Mono Stearate)(2910)以及单油酸甘油酯(Glyceryl Monooleate)(2905)均是购自允诚国际实业有限公司(彰化,台湾地区);十二烷基硫酸钠(Sodium dodecyl sulfate)购自友和贸易股份有限公司(Sigma;Germany)。
仪器设备
1.外压式薄膜乳化设备MG-20(SPG technology;Japan)
2.均质乳化设备Polytron PT2100(Kinematicas;Switzerland)
3.雷射粒径分析仪LS13 320(Beckman coulter;USA)
4.喷雾干燥机L8(Ohkawara;Japan)
5.GC-MS 7890B-5977A(Agilent;USA)
6.回转式震荡恒温培养箱(一升科技;台湾地区)
7.Spectrophotometers V-630(Jasco;Japan)
8.减压浓缩机R-200(Buchi;台湾地区)
预备例1:乳化活性(Emulsion activity;EA)
本预备例以乳化活性(Emulsion activity;EA)筛选合适乳化剂组合。分析方法包括将水、10%大豆油和2.5%的如下表所示的乳化剂组合(HLB值介于11-12.5之间)混合后,以PT2100均质机于11,000rpm条件下进行均质乳化1分钟,再将乳化液以1,500rpm离心20分钟。如果乳化液出现分层现象,立即测量乳化层及总混合液高度,并按照以下公式计算乳化活性: 100×(乳化层高度)/(总混合液高度)。计算结果同样列于下表中。
从上表的结果可以看出乳化剂组合Tween 80/2905具有最佳的乳化活性100%,Tween 20/2905次之(97.1%),Tween 80/2253再次之(94.8%)。在以下实施例即选用乳化剂组合Tween 80/2905(2:1)进行九层塔香精微胶囊的制备。
实施例1
将酪蛋白钠、麦芽糊精、聚山梨醇酯80及十二烷基硫酸钠按照以下表1的重量溶解于水中,并定量至100mL,以转子搅拌混合10-12小时至完全溶解而得到连续相。
将九层塔香精及单油酸甘油酯按照以下表1的重量混合均匀而得到分散相。
表1
原料 | 重量(g) |
九层塔香精 | 20 |
麦芽糊精(Maltodextrin) | 15 |
酪蛋白钠(Sodium Caseinate) | 7 |
聚山梨醇酯80 | 2 |
单油酸甘油酯 | 1 |
十二烷基硫酸钠 | 0.5 |
采用MG-20膜乳化设备,将孔隙大小1.9μm的SPG膜浸于所述连续相当中,以气体压力差增压35-40kPa,将所述分散相挤过SPG膜进入所述连续相中进行乳化,同时于所述连续相中以转子进行400rpm的转动搅拌,转子转动带动的水流将被挤出的分散相带离所述SPG膜,形成分散相 (油滴),平均粒径大小4.7μm的水包油(oil-in-water)乳化液。图1中的实线表示以雷射粒径分析仪LS13 320测量所述水包油乳化液中分散相的粒径的粒径分布结果。
将所述水包油乳化液的一部分以入风温度170℃,及雾化器转速于 19,000rpm的条件下进行喷雾干燥而得到微胶囊粉体。
将前述制备的水包油乳化液的另一部分以高温80℃处理0.5小时后,以雷射粒径分析仪LS13 320测量其中分散相的粒径,粒径分布的结果如图1中的虚线所示,乳化液中分散相(油滴)平均粒径仅小幅增加至4.9μm,粒径变化量仅4.2%。此结果显示本实施例可制备出稳定性佳的九层塔香精乳化液。
实施例2
除了将九层塔香精的用量由20克改成12克外,重复实施例1的步骤制备微胶囊粉体。
实施例3
除了将九层塔香精的用量由20克改成9克,麦芽糊精的用量由15克改成14.5克,及酪蛋白钠的用量由7克改成5克外,重复实施例1的步骤制备微胶囊粉体。
实施例4
将酪蛋白钠、麦芽糊精、***胶、聚山梨醇酯80及十二烷基硫酸钠按照以下表2的重量溶解于水中,并定量至100mL,以转子搅拌混合 10-12小时至完全溶解而得到连续相。
将九层塔香精及单油酸甘油酯按照以下表2的重量混合均匀而得到分散相。
表2
原料 | 重量(g) |
九层塔香精 | 13.5 |
麦芽糊精 | 5 |
酪蛋白钠 | 5 |
***胶(Gum Arabic) | 5 |
聚山梨醇酯80 | 2 |
单油酸甘油酯 | 1 |
十二烷基硫酸钠 | 2 |
重复实施例1的薄膜乳化步骤制备水包油乳化液。
将所述水包油乳化液以入风温度170℃,及雾化器转速19,000rpm的条件进行喷雾干燥,制备出微胶囊粉体。
实施例5
除了将九层塔香精的用量由13.5克改成8克,麦芽糊精的用量由5克改成14克及十二烷基硫酸钠的用量由2克改成1克外,重复实施例4的步骤制备微胶囊粉体。
实施例6
除了将雾化器的入风温度170℃改成150℃外,重复实施例5的步骤制备微胶囊粉体。
实施例7
将酪蛋白钠、麦芽糊精、***胶、聚山梨醇酯80及十二烷基硫酸钠按照以下表3的重量溶解于水中,并定量至100mL,以转子搅拌混合 10-12小时至完全溶解而得到连续相。
将九层塔香精及单油酸甘油酯按照以下表3的重量混合均匀而得到分散相。
表3
原料 | 重量(g) |
九层塔香精 | 12 |
麦芽糊精 | 26 |
酪蛋白钠 | 2.5 |
***胶(Gum Arabic) | 7.5 |
聚山梨醇酯80 | 3 |
单油酸甘油酯 | 1.5 |
十二烷基硫酸钠 | 0.5 |
重复实施例1的薄膜乳化步骤制备水包油乳化液。
将所述水包油乳化液以入风温度120℃,及雾化器转速19,000rpm的条件进行喷雾干燥,制备出微胶囊粉体。
结果
承载率:
承载率为油脂类(精油及乳化剂)在微胶囊粉体占有的比例,以实施例 1来举例,粉体原料总重为45.5克,油重包括九层塔香精、单油酸甘油酯及聚山梨醇酯80,重量为23g。因此,承载率=(23/45.5)x100%=50.5%。
包覆率:
包覆率为粉体内油脂类的含量百分比,以下列公式计算:
包覆率=(1-(表面油重/总油重))x100%
微胶囊粉体表面油重测定:
精确秤取3g微胶囊粉体,置放于砂蕊漏斗中,加入40ml石油醚,轻微搅拌1分钟后进行抽气过滤,再加入25ml石油醚,轻微搅拌40秒后进行抽气过滤,滤液以减压浓缩去除有机溶剂,秤重后得表面油重。
微胶囊粉体总油量测定:
以碱性***提取法测定微胶囊粉体总油量,精确秤取10g微胶囊粉体,以40ml蒸馏水溶解后,加入20ml氨水反应15分钟(以加热器维持65℃反应温度),与40ml乙醇(95%)混合均匀,并于冷水中进行冷却,待溶液冷却后将其转移至分液漏斗,加入40ml***,加塞轻摇及泄气,接着再加入40ml石油醚,剧烈震荡及泄气,静置30分钟后将上清液(醚层) 转入浓缩瓶,减压浓缩去除有机溶剂,秤重后得总油重。
表4
实施例 | 承载率 | 包覆率 |
1 | 50.55% | 86% |
2 | 40.00% | 90% |
3 | 37.50% | 75% |
4 | 49.25 | 18% |
5 | 30.56% | 77% |
6 | 30.25% | 66% |
7 | 31.13% | 45% |
从表4的结果可以看出实施例2-3的酪蛋白钠及麦芽糊精组合在承载率40%及37.5%条件下,包覆率分别为90%以及75%。当实施例1将承载率提高到50%条件时,包覆率则为86%。虽然实施例2具有最高的包覆率 90%,高于实施例1的包覆率,但实施例1的承载率50%高于实施例2的40%。亦即于实施例1中被包覆于微胶囊粉体中的九层塔香精占全部粉体原料的43.47%;实施例2中则只有36%。当以承载率50%进行酪蛋白钠、***胶、麦芽糊精的壁材组合的实验时,如实施例5所示,承载率仅为 18%。因此,在实施例5-7的实验时将承载率下降至约30%,酪蛋白钠、***胶、麦芽糊精的壁材组合可以分别在喷雾干燥温度170℃、150℃及 120℃达成77%、66%及45%的包覆率。以上结果显示,麦芽糊精与酪蛋白钠的组合相较于酪蛋白钠、***胶、麦芽糊精的壁材组合在高承载率条件下具有较高的包覆率。
实施例8:九层塔香精微胶囊稳定性测试
以定子/转子均质乳化技术制作的九层塔香精乳化液作为对照组与实施例1所制造的微胶囊粉体进行比较。定子/转子均质乳化技术使用与实施例1相同的乳化剂制备连续相及分散相,将连续相及分散相均匀混合后,使用PT2100均质机进行均质乳化5分钟(11,000rpm)形成九层塔香精乳化液。最后以与实施例1相同的喷雾干燥技术制备成九层塔香精微胶囊。对照组与实施例1所制造的微胶囊粉体被分装于50ml样品瓶中。于恒温培养箱进行稳定性试验,试验条件如下,恒温60℃储存0、7、14、21、28 及35天(高温***性试验);恒温40℃储存0、14、28、42及56天(高温加速试验),分别检测酸值、硫代巴比妥酸值(TBARS)、油脂包覆率及香气成分。
酸值(Acid value;AV)
精秤10g九层塔香精微胶囊粉末,并以30ml蒸馏水溶解后,加入90 ml正己烷进行油脂萃取2小时,萃取液转移至分液漏斗中,再加入90ml 乙醇(95%)后剧烈震荡及泄气,静置30分钟后,将上清液(醚层)转入浓缩瓶,减压浓缩去除有机溶剂,秤重后得总油重。得到的香精萃取物的酸值按照CNS食用油脂检验法-酸值的测定进行。
硫代巴比妥酸法(Thiobarbituric acid reactive substances;TBARS)
分析方法参考Premanand(Premanand,R.,Santhosh Kumar1,P.H.and Mohan,A.2006.Study of Thiobarbituric Reactive Substances and Total ReducedGlutathione as Indices of Oxidative Stress in Chronic Smokers With andWithout Chronic Obstructive Pulmonary Disease.The Indian Journal of ChestDiseases&Allied Sciences,49:9-11)的方法并加以调整。精秤样品1.5 g,置于15ml离心管,以三氯乙酸(Trichloroacetic acid;TCA)定量至5ml,震摇半小时。3500rpm离心20分钟,吸除油脂后,准确取上清液1ml置于2ml eppendorf内,加入1ml TBA(Thiobarbituricacid;TBA)溶液,混匀并于90℃下反应40分钟,待冷却至室温,以Elisa Reader分光亮度计,检测532nm的吸光值。
香气成分变化
精确秤取10mg九层塔香精微胶囊粉末样品,将其放入20ml玻璃样品瓶中,与3ml蒸馏水混合,加热震荡至完全溶解后,加入10μl内标准品甲醇溶液(p-propyl anisole);另取390mg九层塔香精与60mg乳化剂至 300ml蒸馏水中,以11,000rpm均质1分钟后,取3ml九层塔香精乳化液至20ml玻璃样品瓶中。以Agilent公司的GC Sampler 80进行动态顶部空气自动进样,样品瓶于60℃加热30分钟后,抽取250μl顶部空气进样。挥发性成分以7890B-5977A气相层析质谱仪进行成分分析,使用HP-5MS Ultra Inert毛细管柱(30m×0.25mm×0.20μm);烘箱起始温度40℃停留3 分钟,以每分钟6℃速率升温至250℃并停留5分钟,载气为氦气,管柱气体流量为1mL/min。进样口温度250℃,不分流模式。气相层析质谱仪侦测质量范围为33-400,离子源温度230℃,四极柱温度150℃,电子撞击游离能70eV。以内标准品法计算样品中挥发性成分的相对强度。
酸值
高温加速性试验(40℃)期间,九层塔香精于存放14天内,酸值显著上升,14天之后上升速度趋缓,而九层塔香精微胶囊酸值并无显著上升,其酸值28天后才小幅上升,而后维持数值稳定,显示九层塔香精经过微胶囊包覆,可以有效保护芯材,并延缓其酸值的升高(图2)。高温***性试验(60℃)期间,九层塔香精在7天内酸值显著上升,而九层塔香精微胶囊在21天内酸值无显著变化,28天后酸值才显著上升,显示经过微胶囊包覆的九层塔香精,可以有效延缓或抑制油脂中游离脂肪酸生成(图3)。
TBARS
高温加速性试验(40℃)处理期间,九层塔香精微胶囊的数值稳定持平,而九层塔香精TBARS数值显著上升(图4)。高温***性试验(60℃)期间,九层塔香精TBARS值的上升幅度显著大于九层塔香精微胶囊的TBARS 值(图5)。上述结果显示微胶囊可在高温条件下保护其所包覆的香精物质,有效抑制香精类物质氧化,减少过氧化物的生成,进而达到保护芯材的效果。
香精包覆率变化
九层塔香精微胶囊经过60℃高温***性试验35天后,分析香精包覆率,由86.4%下降至83.0%,共仅下降4%,表示即使在严苛的储存条件下,香精微胶囊型态结构仍可维持完整,被包覆的香精也不易散失;以相同的储存条件参数,均质乳化法制备出的九层塔香精微胶囊,经过相同***性试验35天后,包覆率则由56.7%下降至41.6%,香精包覆率共下降了 15.1%,显示不同的乳化方式会影响壁材包覆的完整性,进而影响香精的包覆率以及产品稳定度(图6)。
风味分子成分变化
以GC-MS检测九层塔香精以及九层塔香精微胶囊的风味分子成分及含量,检测结果显示,风味分子主要为草蒿(Estragole),占所有风味分子 90%以上(图7)。检测经高温***性试验35天后,九层塔香精以及微胶囊的草蒿含量变化,作为风味保留的标的物质。经60℃高温***性试验,九层塔香精风味分子于第35天,风味分子强度下降27%,九层塔香精微胶囊仅下降10%(图8),由此推论,薄膜乳化制备的微胶囊于高温下储存一段时间后,微胶囊型态仍可保持稳定,因此风味物质不容易散失。
以上稳定性测试结果显示,以SPG薄膜乳化搭配喷雾干燥技术制备九层塔香精微胶囊,于贮藏期间香精物质稳定性高、微胶囊结构稳定且风味分子的衰退率低。显示经由薄膜乳化技术,可使风味分子通过多孔玻璃膜形成水包油型乳化液,再经由喷雾干燥技术制备的香精微胶囊可缓慢的释放风味分子,达到控制释放的目的。本发明方法除了应用于九层塔香精,也可用于其他油性风味物质或机能性成分的微胶囊的制备,如鱼油、藻油、卵磷脂、多酚类、黄酮类物质等。
Claims (9)
1.一种油性成分微胶囊制备方法,包含将酪蛋白钠、麦芽糊精与水相乳化剂均匀混合为连续相;将油性成分与油相乳化剂均匀混合为分散相;通过空气压力使所述分散相通过孔隙1.4μm-2.4μm的多孔玻璃膜进入所述连续相,形成粒径均一的乳化液;及将所述乳化液进行喷雾干燥,得到微胶囊粉体。
2.如权利要求1的方法,其中所述多孔玻璃膜的孔隙为约1.9μm。
3.如权利要求1的方法,其中所述水相乳化剂包含聚山梨醇酯80、聚山梨醇酯60或聚山梨醇酯20中的一种,和一种阴离子表面活性剂。
4.如权利要求3的方法,其中所述阴离子表面活性剂为十二烷基硫酸钠。
5.如权利要求4的方法,其中所述水相乳化剂包含聚山梨醇酯80和十二烷基硫酸钠。
6.如权利要求1的方法,其中所述喷雾干燥的入风温度介于120-190℃及出风温度介于80-140℃。
7.如权利要求1的方法,其中所述油性成分包含九层塔香精、鱼油、藻油、卵磷脂、多酚、或黄酮化合物。
8.如权利要求7的方法,其中所述油性成分为九层塔香精。
9.如前述权利要求1至8项中任一项的方法,其中所述油相乳化剂为单油酸甘油酯。
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