CN1250650A - 粉末形式的稳定维生素和类胡萝卜素制剂、和其生产方法 - Google Patents
粉末形式的稳定维生素和类胡萝卜素制剂、和其生产方法 Download PDFInfo
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Abstract
本发明涉及活性成分制剂,其中在蛋白质基质中包埋了一种或多种活性成分,该蛋白质与转谷氨酰胺酶交联。活性成分制剂是例如稳定干燥粉末的形式。本发明另外涉及含有这样的制剂的人类食品和动物饲料,生产该干燥粉末的方法和交联的蛋白质的特定用途。
Description
本发明涉及其中一种或多种活性成分包埋在蛋白质基质中的活性成分制剂。这些蛋白质与转谷氨酰胺酶交联。活性成分制剂的形式例如是稳定的干燥粉末。另外,本发明涉及含有这些制剂的人类食物和动物饲料,生产干燥粉末的方法和交联蛋白质的特定用途。本发明特别涉及含有维生素,人类食物和动物饲料添加剂如类胡萝卜素的干燥粉末。也可能包埋各种添加剂。
粉末形式的维生素和类胡萝卜素产品通常是已知的并且用于大规模的医药工业和人类食品和动物饲料工业中。所以,在文献中叙述了生产稳定产品的许多过程。
叙述了用于生产粉末形式的制剂的各种生产方法特别是喷洒方法,并且其中保护了氧化敏感的物质如可溶于油的维生素或类胡萝卜素以对抗氧化作用。
德国专利1035319叙述了在低湿度含量(低于8%)的大量粉末状淀粉中将油状维生素分散体系喷成雾状。利用干燥淀粉粉末从雾化颗粒除去水。这导致了这些颗粒的固体化,大量淀粉仍然附着于颗粒的表面。这就另外需要除去过量淀粉含量,然后重新用于该方法。
瑞士专利488 455叙述了利用由作为撒粉剂的水推进剂和水吸收物质组成的无机物质。这据说避免了由于精细分裂干燥淀粉存在的爆炸的危险。
瑞士专利389 505公开了在冷的气体介质中将活性成分的分散体系喷成雾状,其中通过冷冻雾化的颗粒固体化。这一过程需要落下的高度是15米,另外温度必须明显保持低于室温。
固体化雾化颗粒的另一个可能的方法是通过把颗粒密封在粉末中,该粉末包括高级脂肪酸的金属盐。这一过程在瑞士专利431 252中叙述了。
在欧洲专利0 618 001中叙述了生产含有稳定活性成分的制剂的可替代方法。在这种方法中,通过控制分散最初从水包油乳化剂形成小球体,其中包括在不可混合水的溶剂中加入油形式的活性成分物质,蛋白质和水,并且然后除去得到的小球体以生产其中活性成分包埋在各种载体物质的混合物中的小球体颗粒。生产小球体必需特定的混合系统。然后,利用醛,例如乙醛,戊二醛或乙二醛处理这种情况中获得的颗粒,导致化学交联,得到物质在水中的不溶性证实了这一点,并且所以获得了活性成分的其它稳定性。
美国专利4 670 247叙述了生产交联颗粒的另一个方法。这可以首先通过喷雾和干燥过程转化乳液成粉末形式的颗粒,乳液基本含有油可溶维生素,保护胶质,例如明胶和还原糖。然后,在热过程中在105和180℃之间处理这些颗粒。由于基质成分的交联,在蛋白质的氨基基团和还原糖的氧基团之间的美拉(Maillard)反应导致干燥粉末颗粒变成不溶于水。
EP 782883叙述了含有胶囊壁并且通过利用可食盐盐析出蛋白质和将胶囊壁与转谷氨酰胺酶交联生产的可食微胶囊。
当对氧化敏感的化合物(在这种情况中特别是脂溶性维生素和类胡萝卜素)与空气接触时,发生了与氧的反应,并且由于转化成不需要的化合物而导致失去活性成分。为了防止这一氧化,例如通过与蛋白质中反应基团反应,依次使它们的氧渗透性更少,并且因此使活性成分得到稳定保护,在制剂中加入一些添加剂是可能的。通过例如在美拉型反应中使蛋白质与还原糖反应,以便防止蛋白质溶解于水中是可以发生的。通过将蛋白质与醛反应获得交联也是可能的,这同样使载体基质的稳定性增加。
但是,这些方法存在一些缺点,以致于寻找提高稳定性的方法似乎是符合需要的。所以,利用在蛋白质和还原糖之间的美拉反应意味着在每种情况下的热应力,并且因此至少在一个小的程度上降解活性成分。另外,证明该产品带棕色。
利用醛作为交联剂与在这种情况中利用对健康特别危险的高反应添加剂的严重缺点相关。这些方法生产的产品没有发现被消费者不受限制的接受。
相反,利用酶交联作为稳定的因素意味着避免了热过程和添加剂,这在每个方面对于每个食物链的天然成分的物质都是无危险的。而且,产品没有棕色。
用本发明的方法生产活性成分的制剂包括下列步骤:
a)完全混合可交联的蛋白质,转谷氨酰胺酶和活性成分的水溶液。
b)喷雾,
其中活性成分和蛋白质之间的比例按重量计是1到10和4到1。
活性成分和蛋白质之间的优选比例按重量计是1到4和2到1,特别优选地是1到3和1到1。
优选的可交联蛋白质是明胶,酪蛋白,大豆蛋白质,玉米蛋白质和胶原。
根据本发明,优选的方法是将含有活性成分的乳液或分散体系喷雾进入装载疏水二氧化硅的惰性气体大气中。
其它优选的方法是喷雾之后干燥残留水分含量低于10%重量,优选地低于6%重量。
本发明的方法的温度基本保持低于80℃,优选地低于602。
本发明另外涉及通过本发明的过程可获得的活性成分制剂以及作为另外的特征,那些活性成分制剂具有释放剂或释放剂混合物的含量是该活性成分的重量的0.025倍到4倍,还涉及含有这一类型的活性成分制剂的人类食品或动物饲料。
优选的释放剂是疏水二氧化硅,玉米淀粉,已经通过化学处理制成疏水的玉米淀粉、高级脂肪酸的金属盐和其它蔬菜淀粉。
在疏水二氧化硅的情况中,活性成分的含量优选地在0.025和0.4范围,特别优选的是0.05和0.2之间。在玉米淀粉的情况中,对应的比例优选地是0.25和2之间,特别优选地在0.5和1.5之间。
通过从碳水化合物和/或天然或化学修饰淀粉的基团生产基本含有这些活性成分,蛋白质和其它载体和膨胀剂的分散体系可获得本发明活性成分制剂。它也可以另外含有添加剂如稳定剂或乳化辅剂。它另外含有能够将蛋白质分子以各种方法连接的酶。由此使蛋白质交联和同时其中包埋活性成分的基质也获得交联,水可溶性减弱,因此增强稳定性。
对于交联基质的分布,获得的活性成分制剂基本是均一的。
优选的可交联蛋白质是明胶,例如骨明胶,小牛明胶,鱼明胶,牛奶蛋白质例如,酪蛋白,大豆蛋白质,玉米蛋白质和胶原,特别优选的蛋白质是牛奶蛋白质和大豆蛋白质。本发明的交联酶是转谷氨酰胺酶,特别是从微生物获得的那些,特别是微生物来源的转谷氨酰胺酶。
优选的活性成分是维生素,和人类食品和动物饲料添加剂。疏水活性成分是特别优选的,以及容易氧化的那些是特别优选的。A,D,E和K组的维生素是这些物质。优选的人类食品和动物饲料添加剂是胡萝卜素和类胡萝卜素,如β-胡萝卜素,和例如虾青素,虾红素,脱-8’-胡萝卜酸乙酯,citranaxanthin鸡油菌黄质,玉米黄素,脱-8’-胡萝卜素,黄体素,辣椒红,番茄红素,和它们的混合物。
利用疏水释放剂如疏水二氧化硅,天然淀粉,例如玉米淀粉,疏水淀粉衍生物,例如疏水玉米淀粉,长链脂肪酸的盐或这些物质的混合物来雾化乳液。但是,释放剂最初也可以存在于喷洒室,例如作为在惰性气体(例如,氮)中的疏水二氧化硅颗粒。然后,通过在空气或保护性气体的蒸汽中处理,适当温和加热到80℃,优选地60℃,特别优选地是在室温,以适当地在除去释放剂之后干燥雾化颗粒。
实施例1
将81.8克明胶(A型100Bloom)和50.7克Isosweet(来自Amylum)分散在360克水中并通过在60℃搅拌30分钟导致溶解。然后加入62.6克玉米淀粉,并且继续搅拌直到所有成分均一分散。接着加入62.9克乙酸维生素A,通过加入乙氧基喹啉(100毫克/106I.U.)和BHT(4.5毫克/106I.U.)使其稳定。利用高效搅拌器在水相中乳化维生素A。最后,加入10%强氢氧化钠水溶液,将得到的乳液的pH调节到8.0,并且与20毫升200单位细菌转谷氨酰胺酶水溶液混合。
然后,在4.2巴的压力下通过单成分管嘴在55℃将得到的乳液喷雾化进入加载疏水二氧化硅的氮气中。然后,在室温下,在15小时内在氮气流中在流体化床干燥器中干燥得到的产品直到残留的水分含量为4.2%。
实施例2
如前面实施例所述来生产干燥粉末,所不同的是没有加入转谷氨酰胺酶。在干燥后,这一产物具有的残留水分含量为3.9%。
实施例3
将来自实施例2的干燥粉末的一部分用120℃的油浴,在旋转烧瓶中热处理20分钟。由于美拉反应产生了棕色颜色。产品的残留水分含量在这一方法中下降到1.9%。
实施例4
通过EP0 065 193中详细叙述的过程生产虾青素配方。
在240克异丙醇以及1.1克抗坏血酸棕榈酸酯和6.4克乙氧喹中悬浮30克虾青素,将压力控制阈值设定在30巴,在混合室中与370克异丙醇连续混合。在悬浮液一边计量速度是6升/小时,在溶剂一边计量值是9升/小时,在混合室设定混合温度为173℃。在0.3秒的停留时间之后,在另一个混合室中调节混合室中的pH到9.5,将分子分散溶液与含有38.6克明胶和105克葡聚糖于4000克水中的溶液以80升/小时的通过量相混合。获得了活性成分的胶质分散体系。颗粒大小分析显示是平均0.15微米,分布范围是±31%。
在薄层薄膜蒸发器中,将微粉粒浓缩到固体含量约25%。然后,浓缩的产品在60℃熔化,加入50毫升250单位细菌转谷氨酰胺酶的水溶液,并且用浆搅拌器在四颈烧瓶中搅拌。
将完成的分散体系导入高温灭菌釜并且通过管嘴喷雾进入含有Sipemat D17作为在空气中分散的喷洒辅剂的容器中。将以这种方式生产的干燥粉末在流化床干燥器中,在20小时内在室温,干燥到水分含量<6%。
实施例5
从得到的干燥粉末中筛选出颗粒大小为250到355微米的部分,在标准预混合物中进行稳定性测试。为此,在样品试管中称重约100毫克测试样品(每个样品,称重和测试4次),然后用手将含有60%小麦麸糠,在二氧化硅上的30%-50%强氯化胆碱和含有37.43%CuSO4×5H2O、46.78%FeSO4×7H2O、11.79%ZnO、3.61%MnO和0.39%CoCO3的10%痕量元素的4克预混合物小心混合。
在恒定温度和湿度(40℃和70%相对湿度)在一厨中的开放容器中储藏测试样品6星期。在储藏开始和4和6星期后,取出用于检测特别测试时间而制备的4个测试样品,并检测其中残留的维生素A活性成分的含量。
测试的结果表示在下面的表中:
维生素A保留(%)
测试产品
干燥粉末 | 起始(I.U./克) | 在4星期后 | 在6星期后 |
1.含有加入的转谷氨酰胺酶 | 494,884 | 86.7 | 79.5 |
2.没有转谷氨酰胺酶 | 520,924 | 85.1 | 76.6 |
3.与2相同,加热处理 | 526,144 | 87.4 | 80.7 |
实施例6
利用420克水,102.3克明胶100Bloom A,63.4克Isosweet,76.5克维生素A乙酸酯(2.16百万I.U./克;利用100毫克乙氧喹/百万I.U.和14.5毫克BHT/百万I.U.来稳定)和80.6克玉米淀粉,如实施例1制备一种乳液,然后利用10%强氢氧化钠水溶液调节该乳液到pH8.0。将这一乳液分成3等分,处理如下:
A:没有加入
B:在多糖中加入2.05克1%强转谷氨酰胺酶制剂(“TG”)。
C:在多糖中加入5.11克强转谷氨酰胺酶制剂(“TG”)。
如实施例1中将乳液喷雾进入用疏水二氧化硅负载的氮气中。
在室温和氮气流中干燥批料A到残留水分含量3.1%。它的一部分在120℃另外加热20分钟。
同样在流体化床中在室温干燥批料B,和在室温将它的一部分储藏后干燥15小时。
如处理批料B那样处理批料C。
将得到的产品如在实施例5中那样进行稳定性测试。将得到的数据归纳在下面的表中。
RT=室温~23℃
产品 | 处理 | 维生素A含量(I.U./克) | 残留水分(%) | 在4星期后残留(%) | 在6星期后残留(%) |
没有加入 | 流化床干燥(=干燥) | 548,700 | 3.1 | 53.9 | 29.1 |
没有加入 | 流化床干燥+热交联 | 563,300 | 1.5 | 63.8 | 45.9 |
2.05克TG | 流化床干燥 | 543,600 | 3.9 | 56.2 | 34.5 |
2.05克TG | RT 15小时+流化床干燥 | 541,900 | 3.4 | 54.8 | 32.4 |
5.11克TG | 流化床干燥 | 540,000 | 3.2 | 62.6 | 35.5 |
5.11克TG | RT15小时+流化床干燥 | 544,600 | 3.6 | 64.4 | 39.7 |
产品 | 处理 | 扩散速度(usec,tau | 强度(kcps) |
没有加入 | 流化床干燥 | 596.3581.2552.2 | 559.3579.0543.3 |
没有加入 | 流化床干燥+热交联 | ||
2.05克TG | 流化床干燥 | 510.7514.6496.9 | 545.4536.4536.4 |
2.05克TG | RT 15小时+流化床干燥 | ||
5.11克TG | 流化床干燥 | 544.0574.4549.5 | 518.3539.1542.3 |
5.11克TG | RT 15小时+流化床干燥 |
明胶是各种大小的蛋白质分子的混合物。利用荧光染料标记所有分子。在观察期,利用广泛的交联,只有最小的分子能够离开交联明胶的网络。另外,较小的分子具有直接受交联的影响的更低的可能性。在与转谷氨酰胺酶广泛交联的明胶的上清液中通过FCS观察分子大小表明通常小分子大小有高扩散速度(在微秒的tau小于对照)。同时观察到所有样品的强度(I,kcps)基本上是相类似的。
实施例7
在另一个测式中,如实施例4将虾青素分散体系加工成为各种量的转谷氨酰胺酶的干燥粉末。
RT=室温~23℃
加入 | 处理 | 活性成分含量(%) | 在6星期后保留物(%) |
没有 | 在RT干燥 | 11,4 | 67 |
0.01%TG | 在RT干燥 | 11,5 | 80 |
0.05%TG | 在RT干燥 | 11,2 | 75 |
Claims (12)
1.生产活性成分制剂的一种方法,该方法包括下列步骤:
a)完全混合可交联的蛋白质,转谷氨酰胺酶和活性成分的水溶液。
b)雾化,
其中在活性成分和蛋白质之间的比例按重量计是1到10和4到1。
2.根据权利要求1的方法,其中活性成分是维生素,人类食品添加剂或动物饲料添加剂。
3.根据权利要求1或2的方法,其中活性成分是疏水的。
4.根据权利要求1到3任一项权利要求的方法,其中可交联蛋白质选自明胶,酪蛋白,大豆蛋白质,玉米蛋白质和胶原。
5.根据权利要求1到4的任一项权利要求的方法,其中利用了从微生物获得的转谷氨酰胺酶。
6.根据权利要求1到5的任一项权利要求的方法,其中发生雾化成为负载疏水二氧化硅,玉米淀粉或疏水玉米淀粉的惰性气体大气。
7.根据权利要求1到6的任一项权利要求的方法,其中雾化后接着干燥到残留水分含量低于10%重量。
8.根据权利要求1到7的任一项权利要求的方法,其中活性成分制剂的温度保持基本上低于80℃。
9.一种活性成分制剂,该制剂由权利要求1到8的任一项权利要求的方法获得。
10.根据权利要求9的活性成分制剂,其中活性成分选自下列一组化合物:
类胡萝卜素
维生素A
维生素E
维生素D3
11.根据权利要求9或10中任一项权利要求的活性成分制剂,其中该活性成分制剂具有释放剂或释放剂混合物的含量是活性成分的重量的0.025到4倍。
12.一种人类食品或动物饲料,其中含有如权利要求9到10的任一项权利要求的活性成分制剂。
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Application Number | Priority Date | Filing Date | Title |
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DE19838189.1 | 1998-08-24 | ||
DE19838189A DE19838189A1 (de) | 1998-08-24 | 1998-08-24 | Stabile pulverförmige Vitamin- und Carotinoid-Zubereitungen und Verfahren zu deren Herstellung |
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CN1250650A true CN1250650A (zh) | 2000-04-19 |
Family
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CN99121688A Pending CN1250650A (zh) | 1998-08-24 | 1999-08-24 | 粉末形式的稳定维生素和类胡萝卜素制剂、和其生产方法 |
Country Status (4)
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EP (1) | EP0982038B1 (zh) |
CN (1) | CN1250650A (zh) |
AT (1) | ATE230612T1 (zh) |
DE (2) | DE19838189A1 (zh) |
Cited By (5)
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CN101600357A (zh) * | 2005-12-08 | 2009-12-09 | 帝斯曼知识产权资产管理有限公司 | 用于活性成分的保护性水胶体 |
CN1764439B (zh) * | 2003-03-27 | 2010-05-26 | 帝斯曼知识产权资产管理有限公司 | 制备交联明胶珠粒的方法 |
CN103327827A (zh) * | 2010-11-26 | 2013-09-25 | 帝斯曼知识产权资产管理有限公司 | 用于活性成分的保护性水胶体 |
CN106173280A (zh) * | 2009-12-09 | 2016-12-07 | 安迪苏法国联合股份有限公司 | 稳定的脂溶性活性成分颗粒 |
CN114698797A (zh) * | 2022-04-29 | 2022-07-05 | 北京宝贝优鲜科技有限公司 | 脱腥鱼肉的制备方法 |
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US6444227B1 (en) * | 1999-08-05 | 2002-09-03 | Roche Vitamins Inc. | Process for preparing fat soluble beadlets |
NL1019931C2 (nl) * | 2002-02-08 | 2003-08-11 | Tno | Verzadiging opwekkend voedingsmiddel. |
FR2836827B1 (fr) * | 2002-03-07 | 2010-10-01 | Innoform Sa | Composition dietetique et cosmetique a base de polymeres naturels reticules immobilisant des actifs |
JP2003259767A (ja) * | 2002-03-11 | 2003-09-16 | Kanro Kk | 疑似餌 |
US6974592B2 (en) | 2002-04-11 | 2005-12-13 | Ocean Nutrition Canada Limited | Encapsulated agglomeration of microcapsules and method for the preparation thereof |
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JP4716982B2 (ja) * | 2003-04-03 | 2011-07-06 | ディーエスエム アイピー アセッツ ビー.ブイ. | 脂溶性活性成分の粉末状配合物 |
US20060159805A1 (en) * | 2003-07-15 | 2006-07-20 | Elger Funda | Powderous formulations of fat-soluble active ingredients |
DE102004041340A1 (de) * | 2004-08-20 | 2006-02-23 | Deutsche Gelatine-Fabriken Stoess Ag | Nanopartikel und Verfahren zu deren Herstellung |
US8034450B2 (en) | 2005-01-21 | 2011-10-11 | Ocean Nutrition Canada Limited | Microcapsules and emulsions containing low bloom gelatin and methods of making and using thereof |
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JPS5828234A (ja) * | 1981-08-08 | 1983-02-19 | Snow Brand Milk Prod Co Ltd | タンパク素材の製造方法 |
US4670247A (en) * | 1983-07-05 | 1987-06-02 | Hoffman-Laroche Inc. | Process for preparing fat-soluble vitamin active beadlets |
JP2897780B2 (ja) * | 1990-03-09 | 1999-05-31 | ニッピゼラチン工業株式会社 | 高重合ゼラチンの製造法 |
JP3012743B2 (ja) * | 1992-09-18 | 2000-02-28 | ニッピゼラチン工業株式会社 | ゼラチン加工食品の製造方法 |
FR2703263B1 (fr) * | 1993-03-31 | 1995-05-19 | Rhone Poulenc Nutrition Animal | Procédé de préparation de sphérules de principes actifs. |
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-
1998
- 1998-08-24 DE DE19838189A patent/DE19838189A1/de not_active Withdrawn
-
1999
- 1999-08-17 EP EP99116089A patent/EP0982038B1/de not_active Expired - Lifetime
- 1999-08-17 AT AT99116089T patent/ATE230612T1/de active
- 1999-08-17 DE DE59903959T patent/DE59903959D1/de not_active Expired - Lifetime
- 1999-08-24 CN CN99121688A patent/CN1250650A/zh active Pending
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Also Published As
Publication number | Publication date |
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EP0982038B1 (de) | 2003-01-08 |
DE19838189A1 (de) | 2000-03-02 |
EP0982038A1 (de) | 2000-03-01 |
DE59903959D1 (de) | 2003-02-13 |
ATE230612T1 (de) | 2003-01-15 |
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