CN111202245A - 维生素d2油脂微胶囊的制备方法、维生素d2油脂微胶囊及其应用 - Google Patents
维生素d2油脂微胶囊的制备方法、维生素d2油脂微胶囊及其应用 Download PDFInfo
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- CN111202245A CN111202245A CN202010066362.6A CN202010066362A CN111202245A CN 111202245 A CN111202245 A CN 111202245A CN 202010066362 A CN202010066362 A CN 202010066362A CN 111202245 A CN111202245 A CN 111202245A
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- vitamin
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Classifications
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Abstract
本发明公开了一种维生素D2油脂微胶囊的制备方法,包括:1)将脂溶性抗氧化剂加入到维生素D2油脂中,再加入水溶性抗氧化剂,混合、剪切;2)将壁材用水溶解;3)将步骤1)得到的混合油脂加入到步骤2)得到的壁材液中,均质;4)将步骤3)得到的液料真空除氧,充入的氮气隔氧;5)采用68‑85℃的温度巴氏杀菌;6)干燥等步骤得到维生素D2油脂微胶囊。本发明还公开了一种维生素D2油脂微胶囊及其在食品中的应用。本发明的方法能够防止生产和存储过程中维生素D2的氧化,保证维生素D2的功效,本发明的维生素D2微胶囊,维生素D2活性高,存储时间长,应用于食品中,能够促进人体钙磷代谢、提高成骨细胞的生理功效。
Description
技术领域
本发明涉及微胶囊,具体涉及一种维生素D2油脂微胶囊的制备方法。本发明还涉及一种维生素D2油脂微胶囊及其在食品中的应用。
背景技术
维生素D2主要来源为植物,其使用的安全性为维生素D3的10-15倍,而在促进人体钙磷代谢、促进成骨细胞的生理功效方面,维生素D2与维生素D3相当。正因为维生素D2的高安全性,其市场前景越来越为人们所认同。
植物来源的维生素D2,主要由蘑菇等真菌经紫外线照射而产生。但蘑菇在干燥后,本身的纤维素结构的溶解性不良,影响了蘑菇中维生素D2的吸收和提取,限制了蘑菇源维生素D2的应用。目前通常采用食用油脂萃取的方法来提取蘑菇中的维生素D2,形成的富含维生素D2的油脂形态的维生素D2产品,并由此增加了蘑菇来源的维生素D2的应用范围。维生素D2的化学名称为“9,10-开环麦角甾-5,7,10(19),22-四烯-3β-醇”,其分子结构中含4个双键,遇光、空气或在湿度大的环境中,容易氧化变质。维生素D2的这一分子结构特点,决定了产品中的维生素D2因氧化而衰减很快,影响了含维生素D2类产品的货架期。
微胶囊技术是指利用成膜材料将固体、液体或气体囊于其中,形成直径几十微米至上千微米的微小容器的技术,微胶囊内部装载的物料称为芯材(或称囊心物质),外部包囊的壁膜称为壁材(或称包囊材料)。经过几十年的不断发展,微胶囊技术已经日趋成熟,被广泛应用在制药、食品、农业化学品、香料、饲料添加剂以及日用化学品等工业领域。因微胶囊化后,油脂的热敏性和光敏性降低,从而可防止脂溶性成分受到破坏。同时,油脂微胶囊将油脂制品包裹在壁材中,减轻了油脂食用时的油腻感,改善了食用的口感。微胶囊的微粒化结构也提供了油脂产品的生物利用度。
现有微胶囊的生产方法中,为了保护油脂中的易氧化有效成分,降低氧化程度,多采用缩短工艺流程、于壁材中添加水溶性抗氧化剂的方式予以生产。即先将壁材、水溶性抗氧化剂溶解,后加入不饱和油脂或保健功效成分的工艺。在这一工艺过程中,虽然缩短了工艺处理流程,但因为在壁材等的溶解过程中,溶液的温度较高、抗氧化剂的损失较多;抗氧化剂的浓度易因壁材的稀释而下降,不能有效保护后期加入的易氧化有效成分;微胶囊溶液在均质过程中混入一定的氧。这些都导致了微胶囊生产过程中氧化损失较高,存储阶段对易氧化有效成分的保护作用下降。
发明内容
本发明所要解决的技术问题是提供一种维生素D2油脂微胶囊的制备方法,能够减少生产过程中维生素D2的损失,延长产品的保质期。
本发明还要解决的技术问题是提供一种维生素D2油脂微胶囊,适口性好,保质期长。
本发明进一步所要解决的技术问题是提供一种维生素D2油脂微胶囊的应用。
为了实现上述目的,本发明一方面提供一种维生素D2油脂微胶囊的制备方法,包括如下步骤:1)将脂溶性抗氧化剂用植物油或酒精溶解后,加入到维生素D2油脂中,再加入用纯净水溶解后的水溶性抗氧化剂,混合、剪切;2)将壁材用水溶解;3)将步骤1)得到的混合油脂加入到步骤2)得到的壁材液中,均质;4)将步骤3)得到的液料真空除氧,充入氮气隔氧,暂存;5)采用68-85℃的温度巴氏杀菌;6)干燥,得到维生素D2油脂微胶囊。
根据本发明,在所述步骤1)中,所述脂溶性抗氧化剂可以为本领域常规使用的各种脂溶性抗氧化剂,优选地,所述脂溶性抗氧化剂选自卵磷脂、L-抗坏血酸棕榈酸酯、维生素E、BHA、BHT和TBHQ中的至少一种。所述脂溶性抗氧化剂的添加量的可选择范围较宽,优选情况下,为了更好地实现本发明的发明目的,所述脂溶性抗氧化剂的添加量为配料总重量的的100-4000ppm。在该优选技术方案中,卵磷脂、L-抗坏血酸棕榈酸酯、维生素E、BHA(丁基羟基茴香醚)、BHT(二丁基羟基甲苯)和TBHQ(特丁基对苯二酚)均为安全性较高,可用于食品的脂溶性抗氧化剂,能够溶解于植物油和酒精。其中的卵磷脂既具有抗氧化作用,又具有较高的营养价值;L-抗坏血酸棕榈酸酯和维生素E均具有一定的营养价值。100-1500ppm的浓度既能够起到防止维生素D2油脂中的维生素D2氧化的作用,又符合国家的安全标准。用于溶解所述脂溶性抗氧化剂的植物油可以为本领域常规使用的各种植物油,优选地,所述植物油为葵花籽油、菜籽油和大豆油中的至少一种。葵花籽油、菜籽油和大豆油能够有效地溶解脂溶性抗氧化剂,使得脂溶性抗氧化剂均匀分散到维生素D2油脂中,其本身也具有营养价值。
根据本发明,在所述步骤1)中,所述水溶性抗氧化剂可以为本领域常规使用的各种水溶性抗氧化剂,优选地,所述水溶性抗氧化剂为L抗坏血酸和/或L抗坏血酸钠;所述水溶性抗氧化剂的添加量为配料总重量的1-4%。L抗坏血酸和L抗坏血酸钠抗氧化作用强,水溶性好。其中的L抗坏血酸钠为中性,不会增加维生素D2油脂的酸度。
进一步优选地,在所述水溶性抗氧化剂中,还加入抗氧化剂增效剂,所述抗氧化剂增效剂为柠檬酸和/或柠檬酸钠,所述抗氧化剂增效剂的添加量为配料总重量的0.05-0.1%。通过该优选技术方案,抗氧化剂增效剂柠檬酸或柠檬酸钠与抗氧化剂混合使用,能够有效地提高抗氧化作用,提高维生素D2油脂的保质期。
根据本发明,在所述步骤2)中,所述壁材可以为本领域常规使用的各种壁材,优选地,所述壁材选自麦芽糊精、固体玉米糖浆、葡萄糖和淀粉中的至少一种,所述壁材的使用量为配料总重量的43-64%。在该优选技术方案中,使用麦芽糊精、固体玉米糖浆、葡萄糖和淀粉中的至少一种作为壁材,能够对维生素D2油脂形成更好地包裹,形成的微胶囊颗粒更均匀。占配料总重量43-64%的壁材用量,包埋率高,表面油脂含量低,食用时更易于溶解吸收。
优选地,在所述步骤2)中,还加入乳化剂,所述乳化剂为酪朊酸钠、酪朊酸钾、辛烯基琥珀酸淀粉钠和乳清蛋白粉中的至少一种,所述乳化剂的添加量为配料总重量的3.5-16.5%。在该优选技术方案中,乳化剂的加入使得维生素D2油脂更容易分散到壁材溶液中,形成微小的水包油乳剂。形成的微胶囊粒径更小,更均匀。
优选地,在所述步骤3)中,所述均质的压力为20-100Mpa。通过该优选技术方案,能够使得维生素D2油脂均匀的分散到壁材溶液中,形成均一的乳化液。
根据本发明,在所述步骤4)中,可以充入惰性气氛进行隔氧,所述惰性气氛可以为化学性质比较稳定的气体,如元素周期表零族气体、氮气等。为了方便操作并节约成本,所述惰性气氛为氮气。对氮气的纯度没有特别限定,但是优选情况下,所充入氮气的纯度为99.9-99.999%。在该优选技术方案中,99.9-99.999%的氮气中含有的氧气更少,能够更好地使得乳化液与空气中的氧气隔绝,乳化液中的残氧更少,在加工和保存过程中维生素D2更不容易被氧化而遭到破坏。
优选地,在所述步骤6)中,在所述微胶囊中还加入抗结剂,所述抗结剂为磷酸三钙,所述抗结剂的添加量为配料总重量的0.1-0.2%。通过该优选技术方案,抗结剂能够使得干燥后的微胶囊形成松散的粉末状而不易结块,方便微胶囊的使用和溶解吸收。
本发明第二方面提供了一种根据本发明所述的方法制得的维生素D2油脂微胶囊,该维生素D2微胶囊的表面油≤0.4%,过氧化值≤3meq/kg。
本发明第三方面提供了本发明所述的维生素D2油脂微胶囊在健康食品、保健食品中的应用。
通过上述技术方案,本发明的维生素D2油脂微胶囊的制备方法,在维生素D2油脂中同时使用了脂溶性抗氧化剂和水溶性抗氧化剂,抗氧化效果更好。在加工过程中采用隔氧措施,特别是在高温工序中的隔氧措施,有效地防止了维生素D2在微胶囊加工过程中的氧化损失。本发明的维生素D2微胶囊,包埋率高,表面油量低,有效存储时间长。本发明的维生素D2微胶囊能够应用在软胶囊、凝胶糖果、压片糖果、固体饮料等健康食品,以及婴幼儿配方食品和保健食品中。
具体实施方式
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值,这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说,各个范围的端点值之间、各个范围的端点值和单独的点值之间,以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围,这些数值范围应被视为在本文中具体公开。
以下通过具体实施例对本发明的技术方案进行详细描述。以下实施例中所采用的水是通过反渗透法制得的纯净水。剪切机采用德国弗鲁克生产的FDC1/60在线高剪机。其他原料、设备、试剂均为普通市售产品。产品中成分的检测均按照国标中的规定进行测定。
实施例1
步骤1:称取1g卵磷脂、6g维生素E,加入20g葵花籽油中,搅拌,完全溶解后,加入到1.25Kg含5300IU/g维生素D2的维生素D2油脂中。
称取125g抗坏血酸钠,25g柠檬酸钠,加入300g纯净水溶解后,加入上述维生素D2油脂中,使用剪切机以6000rpm的转速混合,剪切10分钟。
步骤2:称取1.916Kg固体玉米糖浆、0.9Kg麦芽糊精,750g辛烯基琥珀酸淀粉钠,加入4Kg纯净水,搅拌至完全溶解。
步骤3:将步骤2得到的溶液(水相)加入到均质暂存罐中,再加入步骤1得到的混合油脂(油相),采用50MPa的压力均质2次,得到维生素D2乳化液。
步骤4:将维生素D2乳化液加入料液暂存罐中,在-0.09Mpa的压力下真空除氧10分钟,再充入纯度为99.99%的氮气隔氧。
步骤5:将维生素D2乳化液采用在线巴氏杀菌的方式进行杀菌:使用在线巴氏杀菌器,杀菌温度为76-82℃、料液在巴氏杀菌器中停留时间2分钟。
步骤6:、将杀菌后的维生素D2乳化液采用压力喷雾干燥法干燥,喷雾塔热风温度175-180℃。在干燥后的粉末中加入7g的磷酸三钙,搅拌均匀,得到成品维生素D2油脂微胶囊。
实施例2
步骤1:称取7g L-抗坏血酸棕榈酸酯、13g维生素E,加入20g菜籽油中,搅拌,完全溶解后,加入到1.325Kg含4800IU/g维生素D2的维生素D2油脂中。
称取200g L抗坏血酸钠,50g柠檬酸钠,加入400g纯净水溶解后,加入上述维生素D2油脂中,使用剪切机以6000rpm的转速混合,剪切10分钟。
步骤2:称取3.2Kg固体玉米糖浆,175g酪朊酸钠,加入5Kg纯净水,搅拌至完全溶解。
步骤3:将步骤2得到的溶液(水相)加入到均质暂存罐中,再加入步骤1得到的混合油脂(油相),采用100MPa的压力均质2次,得到维生素D2乳化液。
步骤4:将维生素D2乳化液加入料液暂存罐中,在-0.07Mpa的压力下真空除氧15分钟,再充入99.99%的氮气隔氧。
步骤5:将维生素D2乳化液采用在线巴氏杀菌的方式进行杀菌:使用在线巴氏杀菌器,杀菌温度为80-85℃、料液在巴氏杀菌器中停留时间2分钟。
步骤6:、将杀菌后的维生素D2乳化液采用压力喷雾干燥法干燥,喷雾塔热风温度175-180℃。在干燥后的粉末中加入10g的磷酸三钙,搅拌均匀,得到成品维生素D2油脂微胶囊。
实施例3
步骤1:称取0.5g BHT,加入10g酒精中,搅拌,完全溶解后,加入到1.967Kg含3250IU/g维生素D2的维生素D2油脂中。
称取50g L抗坏血酸钠,2.5g柠檬酸,加入200g纯净水溶解后,加入上述维生素D2油脂中,使用剪切机混合,剪切10分钟。
步骤2:称取2.15Kg固体玉米糖浆,475g辛烯基琥珀酸淀粉钠,350g乳清蛋白粉,加入5Kg纯净水,搅拌至完全溶解。
步骤3:将步骤2得到的溶液(水相)加入到均质暂存罐中,再加入步骤1得到的混合油脂(油相),采用20MPa的压力均质2次,得到维生素D2乳化液。
步骤4:将维生素D2乳化液加入料液暂存罐中,在-0.06Mpa的压力下真空除氧5分钟,再充入99.99%的氮气隔氧。
步骤5:将维生素D2乳化液采用在线巴氏杀菌的方式进行杀菌:使用在线巴氏杀菌器,杀菌温度为68-72℃、料液在巴氏杀菌器中停留时间2分钟。
步骤6:将杀菌后的维生素D2乳化液采用压力喷雾干燥法干燥,喷雾塔热风温度175-180℃。在干燥得到的粉末中加入5g的磷酸三钙,搅拌均匀,得到成品维生素D2油脂微胶囊。
实施例4
步骤1:称取1g TBHQ,加入10g大豆油中,搅拌,完全溶解后,加入到1.804Kg含3400IU/g维生素D2的维生素D2油脂中。
称取175g L抗坏血酸、5g柠檬酸,加入300g纯净水溶解后,加入上述维生素D2油脂中,使用剪切机以6000rpm的转速混合,剪切10分钟。
步骤2:称取3Kg葡萄糖,加入5Kg纯净水,搅拌至完全溶解。
步骤3:将步骤2得到的溶液(水相)加入到均质暂存罐中,再加入步骤1得到的混合油脂(油相),采用30MPa的压力均质3次,得到维生素D2乳化液。
步骤4:将维生素D2乳化液加入密闭容器中,在-0.08Mpa的压力下真空除氧10分钟,再充入99.999%的氮气隔氧。
步骤5:将维生素D2乳化液采用在线巴氏杀菌的方式进行杀菌:使用在线巴氏杀菌器,杀菌温度为72-76℃、料液在巴氏杀菌器中停留时间2分钟。
步骤6:将杀菌后的维生素D2乳化液采用压力喷雾干燥法干燥,喷雾塔热风温度175-180℃。在干燥得到的粉末中加入5g的磷酸三钙,搅拌均匀,得到成品维生素D2油脂微胶囊。
实施例5
步骤1:称取2g的BHA,加入10g酒精中,搅拌,完全溶解后,加入到1.913Kg含3290IU/g维生素D2的维生素D2油脂中。
称取75g L抗坏血酸钠,10g柠檬酸,加入300g纯净水溶解后,加入上述维生素D2油脂中,使用剪切机混合,剪切15分钟。
步骤2:称取2.5Kg淀粉,500g酪朊酸钾,加入5Kg纯净水,搅拌至完全溶解。
步骤3:将步骤2得到的溶液(水相)加入到均质暂存罐中,再加入步骤1得到的混合油脂(油相),采用80MPa的压力均质,得到维生素D2乳化液。
步骤4:将维生素D2乳化液加入密闭容器中,在-0.06Mpa的压力下真空除氧10分钟,再充入99.9%的氮气隔氧。
步骤5:将维生素D2乳化液采用在线巴氏杀菌的方式进行杀菌:使用在线巴氏杀菌器,杀菌温度为76-82℃、料液在巴氏杀菌器中停留时间2分钟。
步骤6:将杀菌后的维生素D2乳化液采用压力喷雾干燥法干燥,喷雾塔热风温度175-180℃,得到成品维生素D2油脂微胶囊。
对照例
步骤1:称取1.835Kg固体玉米糖浆、0.9Kg麦芽糊精,750g辛烯基琥珀酸淀粉钠、200g L抗坏血酸钠,加入6kg纯净水,搅拌至完全溶解。
步骤2:将步骤1得到的溶液(水相)加入到均质暂存罐中,再加入1.31Kg含4710IU/g维生素D2的维生素D2油脂(油相),采用100MPa的压力均质,得到维生素D2乳化液。
步骤3:将维生素D2乳化液加入密闭容器中,在-0.09Mpa的压力下真空除氧10分钟,再充入99.9%的氮气隔氧。
步骤4:将维生素D2乳化液采用在线巴氏杀菌的方式进行杀菌:使用在线巴氏杀菌器,杀菌温度为76-82℃、料液在巴氏杀菌器中停留时间2分钟。
步骤5:将杀菌后的维生素D2乳化液采用压力喷雾干燥法干燥,喷雾塔热风温度175-180℃。在干燥得到的粉末中加入5g的磷酸三钙,搅拌均匀,得到成品维生素D2油脂微胶囊。
对上述各实施例和对照例中得到的维生素D2油脂微胶囊,分别检测其表面油、维生素D2含量和过氧化氢值。得到的检测值见表1。由表1可以看出,本发明的维生素D2油脂微胶囊的制备方法,加工过程中维生素D2的损失小,表面油含量低,适口性好。
表1各实施例得到的维生素D2油脂微胶囊检测数据
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对照例 | |
维生素D<sub>2</sub>添加量(IU/g) | 1300 | 1272 | 1280 | 1230 | 1258 | 1234 |
维生素D<sub>2</sub>检测量(IU/g) | 1268 | 1240 | 1200 | 1154 | 1109 | 1095 |
表面油含量(%) | 0.25 | 0.28 | 0.3 | 0.35 | 0.29 | 0.51 |
将各实施例得到的维生素D2油脂微胶囊存放一年,并分别在存放1周、1月、6月、1年时检测其维生素D2含量和过氧化氢值。得到的结果见表2。
表2各实施例得到的维生素D2油脂微胶囊存放指标
从表2的数据可以看出,本发明的维生素D2油脂微胶囊,存放过程中维生素D2含量的损失较小,过氧化值的提高较慢,经过1年的存放后其过氧化值仍小于3meq/kg。有效保存期限长,具有更长的保质期。
使用本发明的维生素D2油脂微胶囊制成的软胶囊、凝胶糖果、压片糖果、固体饮料等健康食品,以及婴幼儿配方食品、中老年配方食品等普通食品,含有足量的维生素D2,能够供使用者补充维生素D。且适口性好,货架期长。
以上详细描述了本发明的优选实施方式,但是,本发明并不限于此。在本发明的技术构思范围内,可以对本发明的技术方案进行多种简单变型,包括各个技术特征以任何其它的合适方式进行组合,这些简单变型和组合同样应当视为本发明所公开的内容,均属于本发明的保护范围。
Claims (10)
1.一种维生素D2油脂微胶囊的制备方法,其特征在于,包括如下步骤:
1)将脂溶性抗氧化剂用植物油或酒精溶解后,加入到维生素D2油脂中,再加入用纯净水溶解后的水溶性抗氧化剂,混合、剪切;
2)将壁材用水溶解;
3)将步骤1)得到的混合油脂加入到步骤2)得到的壁材液中,均质;
4)将步骤3)得到的液料真空除氧,充入氮气隔氧,暂存;
5)采用68-85℃的温度巴氏杀菌;
6)干燥,得到维生素D2油脂微胶囊。
2.根据权利要求1所述的方法,其特征在于,在所述步骤1)中,所述脂溶性抗氧化剂为卵磷脂、L-抗坏血酸棕榈酸酯、维生素E、BHA、BHT和TBHQ中的至少一种,所述脂溶性抗氧化剂的添加量为配料总重量的100-4000ppm;
所述植物油为葵花籽油、菜籽油和大豆油中的至少一种;
所述水溶性抗氧化剂为L抗坏血酸和/或L抗坏血酸钠;所述水溶性抗氧化剂的添加量为配料总重量的1-4%。
3.根据权利要求2所述的方法,其特征在于,在添加所述水溶性抗氧化剂时,还加入抗氧化剂增效剂,所述抗氧化剂增效剂为柠檬酸和/或柠檬酸钠,所述抗氧化剂增效剂的添加量为配料总重量的0.05-1%。
4.根据权利要求1所述的方法,其特征在于,在所述步骤2)中,所述壁材选自麦芽糊精、固体玉米糖浆、葡萄糖和淀粉中的至少一种,所述壁材的使用量为配料总重量的43-64%。
5.根据权利要求1所述的方法,其特征在于,在所述步骤2)中,还加入乳化剂,所述乳化剂为酪朊酸钠、酪朊酸钾、辛烯基琥珀酸淀粉钠和乳清蛋白粉中的至少一种,所述乳化剂的添加量为配料总重量的3.5-16.5%。
6.根据权利要求1所述的方法,其特征在于,在所述步骤3)中,所述均质的压力为20-100MPa。
7.根据权利要求1所述的方法,其特征在于,在所述步骤4)中,所充入氮气的纯度为99.9-99.999%。
8.根据权利要求1所述的方法,其特征在于,在所述步骤6)中,在所述微胶囊中还加入抗结剂,所述抗结剂为磷酸三钙,所述抗结剂的添加量为配料总重量的0.1-0.2%。
9.一种维生素D2油脂微胶囊,其特征在于,根据权利要求1至8中任一项所述的方法制得,该维生素D2微胶囊的表面油≤0.4%,过氧化值≤3meq/kg。
10.权利要求9所述的维生素D2油脂微胶囊在婴幼儿配方食品、健康食品、保健食品中的应用。
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