CN1165245C - 醋蛋粉的制造方法 - Google Patents
醋蛋粉的制造方法 Download PDFInfo
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- CN1165245C CN1165245C CNB998016594A CN99801659A CN1165245C CN 1165245 C CN1165245 C CN 1165245C CN B998016594 A CNB998016594 A CN B998016594A CN 99801659 A CN99801659 A CN 99801659A CN 1165245 C CN1165245 C CN 1165245C
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- egg
- acid
- vinegar
- shell
- edibility
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Abstract
本发明提供一种醋蛋粉的制造方法,其特征是,按照本发明,往全蛋(包括蛋壳)中添加可食性酸水溶液,对全蛋100g,其添加量至少为150ml,于约0~约50℃的温度浸渍处理所得到的醋蛋溶液,根据场合,过滤后,在吹入温度180℃以上、排气温度120℃以上的条件下进行喷雾干燥,或者,往全蛋(包括蛋壳)里添加可食性水溶液及水解酶,于约0~约50℃的温度进行分解处理,把所得到的分解物生成液,根据场合,进行加热灭菌处理及/或过滤后,加以干燥,制成粉末。
Description
技术领域
本发明涉及新型的醋蛋粉的制造方法。更详细地说,涉及具有芳香味并且醋酸味极少的富于嗜好性的醋蛋粉,以及,涉及消化性优异并且产生蛋变应性少的醋蛋粉的制造方法。
背景技术
早先,醋蛋一般是通过往蛋中加醋,放置5~10天制造出来的,供直接食用,然而,不仅制造需要长时间,而且,食味和食感也不理想,不能长期保存,也难以随时摄取。也就是说,把全蛋放入容器,添加食用醋浸渍,于室温放置5~10天,使蛋壳溶于食用醋后,以溶解的蛋壳作为酸化钙及酸化矿物盐液体,用搅拌器把该液体与蛋膜中的蛋白和蛋黄部分一起加以混合,以该全蛋溶液作为保健饮料,每次饮用10~20ml,然而,可溶化的酸化钙及作为其他成分的镁、钾、铝、锰、铁、硒、锌等矿物,构成可溶于水的酸化矿物盐状态时,相当苦,另外,还有辣嗓子味感觉,此外,加之还有酸味,特别难以饮用。然而,当保存期限长到1~2个月后,经常发生腐败变质。另外,上述醋蛋溶液,原样状态下杂菌很多,然而,当进行加热灭菌处理时,产生凝固(因蛋白质发生凝固),所以作饮料不合适。
自古以来,醋蛋是作为保健食品使用的,作为改良了上述缺点的醋蛋制品及其制造方法,已公开的有,例如,把生蛋浸渍在柠檬酸或苹果酸水溶液中,蛋壳溶解后,搅拌蛋白、蛋黄,加以混合,制成醋蛋类食品(特公昭55-33号公报);把蛋壳溶于食用醋等中,往混入了自芝麻的酸溶液中加入蛋白、蛋黄等蛋液,制成醋蛋,其中亚油酸对蛋黄的胆甾醇(コレスト口-ル)1份的比例达到2份(特开昭61-158764号公报);磷对钙的重量比为2以上的含醋蛋食品(特开昭61-234758号公报);往干燥的蛋壳粉中添加食用醋和其他有机酸溶液,使其溶解,过滤后,与蛋液加以混合的醋蛋制造方法(特公昭63-45793号公报);在干燥的蛋白、干燥的蛋黄和蛋壳粉中,混合醋粉,有机酸和调料,制造固体醋蛋的方法(特公昭63-47438号公报);把蛋壳粉溶于食用醋或有机酸溶液后,制成干燥粉状的醋蛋类营养食品的制造方法(特开昭61-185168号公报);把鸟类的全蛋或蛋壳浸渍在醋液中制造醋蛋时,添加抗坏血酸、β-胡罗卜素,再使其吸附在麦芽糖上,冷冻干燥制成的保健食品及其制造方法(特开平8-38107号公报)、含有抗坏血酸的醋蛋冻胶食品(特开平8-80174号公报);含乌骨鸡提取物的醋蛋冻胶食品(特开平8-80175号公报);在醋蛋中混合干燥的蘑菇、炒过的大豆、干燥的海带、延命草、炒过的芝麻、炒过的米糠、柿子叶等构成的醋蛋类混合食品(特开平8-214834号公报)、脱脂醋蛋粉(特许第2707511号)等。
早先公开的这些醋蛋及其制造方法,对醋蛋制造工序进行了改变,但是,所得到的醋蛋,任何一种其消化吸收性能均不理想,而且,酸味强,相当苦,嗜好性差,还可能产生蛋的变应性。
本发明人等,为了改善把可食性酸水溶液添加至全蛋中制造的醋蛋的嗜好性差的缺点进行了悉心探讨,结果发现,把可食性酸水溶液添加至全蛋中制成的醋蛋溶液在特定的条件下加以喷雾干燥时,蒸发去除过剩而残留的可食性酸,同时,适当焙煎蛋的组成成分,得到具有理想的香味,极富于嗜好的醋蛋粉。
而且,本发明人等在通常的状态下,把生物吸收性差的蛋壳,与蛋白和蛋黄一起,制成易于溶化吸收的状态,并改善醋蛋饮用的不宜性,为使含蛋壳的全蛋成分具有优良的生物吸收性进行反复悉心研究的结果发现,把全蛋用可食性酸类进行溶化处理时,如同时使用能使蛋白质、脂肪、碳水化合物水解的酶时,可促进全蛋成分的分解(消化)和溶化,在谋求缩短醋蛋生产周期的同时,将所得到的醋蛋的消化吸收性显著提高,而且,还能抑制蛋变应性的发生。
发明的公开
因此,按照本发明的第一实施方案,提供一种制造具有香味且无醋味的,嗜好性丰富的醋蛋粉的方法,该法的特征是,往100g全蛋(包括蛋壳)里至少加150ml比例的可食性酸水溶液,于约0~约50℃的温度下进行浸渍处理,把如此得到的醋蛋溶液,根据场合,过滤后,在吹入温度在180℃以上、排气温度在120℃以上的条件下,进行喷雾干燥。
按照本发明的第二实施方案,提供一种醋蛋粉的制造方法,其特征是往全蛋(包括蛋壳)中添加可食性酸水溶液以及水解酶,于约0~约50℃的温度下加以分解处理,把所得到的分解物生成液,根据场合,进行加热灭菌处理及/或过滤后,进行干燥,制成粉,特别理想的是在吹入温度为180℃以上、排气温度为120℃以上的条件下进行喷雾干燥。
下面将更加详细地说明本发明的方法。
本发明的实施方案
在本发明的方法中,作为原料使用的蛋,鸡蛋(普通蛋、受精蛋和碘蛋等)是理想的,但是,其他的蛋,例如,鸭蛋及鹌鹑蛋等以及其他的鸟类的蛋,也同样可以使用。在本发明中,不仅蛋白和蛋黄,而且,包括蛋壳在内的全蛋成分也可用作原料。
在本发明的第一实施方案中,首先,把包括蛋壳在内的全蛋浸渍在可食性酸水溶液中进行溶解处理。该溶解处理,是在约0~约50℃的温度,通常是在室温和大气压条件下,使原料全蛋与可食性酸水溶液充分接触来进行。此时,为了促进蛋壳的溶解,也可进行适当搅拌。浸渍处理要进行到至少是大部分蛋壳已溶解,蛋壳固体成分几乎消失为止。因此,通常要5~10天。
另外,按照本发明的第二实施方案,把可食性酸水溶液及水解酶加至含蛋壳的全蛋中,也可进行全蛋成分的分解处理。此时,水解酶可与可食性酸水溶液一起加至全蛋中,或者,先把可食性醋溶液加至全蛋中进行分解处理,在蛋壳溶解至某种程度时,例如,在蛋壳已部分溶解的阶段,或在蛋壳实质上已完全溶解的阶段,根据场合,用搅拌器进行破碎处理,形成破碎的乳液后,加入水解酶,再次进行分解处理也可以,或者,最初就用搅拌器等把全蛋进行破碎处理,配制成全蛋破碎乳液,把可食性酸水溶液及水解酶添加至上述破碎乳液中,进行分解处理。
分解处理,在约0~约50℃的温度下,通常在室温和大气压的条件下,使原料全蛋与可食性酸水溶液及水解酶充分接触来进行。分解处理进行到至少是蛋壳的大部分已溶解,即蛋壳的固体成分几乎消失为止。理想的是蛋壳的大部分溶解后,至少还要继续1~2天。
分解处理时间,可根据原料蛋的种类,与所用的可食性的酸水溶液的接触状态、分解处理的条件等自由改变,但是,通过并用水解酶,一般1~3天左右就足够了,在不使用水解酶的场合,须要5~10天左右,两者比较,处理时间可大大缩短。
作为本发明中使用的可食性酸水溶液,可以举出,例如,米醋、黑醋、苹果醋等酿造的或合成的食用醋;醋酸、苹果酸、柠檬酸、琥珀酸和乳酸等可食性有机酸的水溶液,这些可分别单独使用,也可两种以上组合起来使用。这些可食性酸水溶液,其pH值的范围一般为1~5,理想的为2~4。
对上述可食性酸水溶液的用量,未作严格限制,可根据其种类,以及与全蛋的接触状态,是否使用水解酶等来加以改变,例如,在主要成分为醋酸等有机酸的情况下,一般是对每100g全蛋,至少用100ml,特别是用150~500ml,更特别是用200~400ml的比例是合适的。
另外,根据场合,作为与可食性酸水溶液一起用的水解酶,可使用具有能使蛋白质、脂肪和碳水化物等有水解能力的、从市场购得的各种酶制剂,具体的可以举出,例如,肌酸酶(クラィスタ-ゼ)(大和化成(株)制)、生物淀粉酶、根霉菌属酶、脂肪酶、胰酶制剂(以上为天野制药(株)制)、胃蛋白酶(ミクニ化学产业(株)制)、卵磷脂酶10L(ノボノルディスクバィォィンダストリ-(株)制)等。对这些酶制剂的用量也未作严格限制,可根据原料蛋的种类及分解处理条件等加以改变,但是,通常对每100g全蛋用0.01~1g,特别是使用0.02~0.5g是合适的。
通过这种酶制剂的使用,可促进占蛋壳约93%以上的碳酸钙、其他含少量的碳酸镁、磷酸钙等无机物结晶间的蛋白质、由多糖等构成的粘结成分的分解,通过可食性酸的作用,蛋壳钙的水溶化加快,另外,蛋白和蛋黄中的蛋白质及脂质、糖质的分解也被促进,成为低分子量,从而生物吸收性得到格外的提高,结果是,所得到的全蛋分解物生成液具有,即使通过灭菌处理所必须的60~80℃进行热处理也不发生凝固,另外,即使在进行喷雾干燥时,实际上也不发生变质等各种优良的特性。
通过上述溶解处理或分解处理得到的醋蛋溶液或全蛋分解物生成液,根据场合,用常规方法进行加热灭菌处理及/或进行酶失活处理,及/或通过过滤等去除残留的固体成分,然后,干燥,制成粉末。
在本发明的第二实施方案中的分解物生成液的干燥粉末化,可以采用该领域已知的方法,例如,喷雾干燥、冷冻干燥和减压浓缩等方法来进行,然而,其中,喷雾干燥是优选的。
喷雾干燥,可采用通常的喷雾干燥装置进行实施。在本发明的第一实施方案的特征在于,其操作条件特别是吹入温度设定在180℃以上,理想的是190~230℃;而排气温度设定在120℃以上,理想的是在120~170℃的较高温度,由此,残留的过剩的可食性酸,尤其是醋酸可被蒸发去除,同时,由于该喷雾干燥条件下,通过焙煎作用,可赋予蛋的组成成分以芳香,使所得到的醋蛋粉富于极大的嗜好性。
还有,上述醋蛋溶液或全蛋分解物生成液,在进行干燥粉末化,例如,在喷雾干燥阶段,希望pH值为5~8,特别希望在5.5~7的范围内,在该阶段,如pH值不在上述范围内,则优选通过可食性酸或碱调节pH值进入上述范围内。
另外,在本发明的方法的任意阶段,特别是在通过可食性酸水溶液浸渍全蛋、溶解处理工序或通过水解酶的分解处理的初期工序,或者在干燥前的工序,往全蛋溶解液或分解液中添加蛋壳粉、碳酸钙、醋酸钙、乳酸钙等钙源,则可以得到富钙的醋蛋粉。这种钙源的添加量,一般是对每100g原料蛋,作为钙为1~10g,特别是在1~5g的范围是理想的。
而且,在上述醋蛋溶液的喷雾干燥或分解物生成液的干燥粉末化时,优选的是,可以配合适当的赋形剂或添加剂。作为所用的赋形剂或添加剂,可以举出,例如明胶、胶原蛋白、酪蛋白、蛋的白蛋白、阿拉伯树胶、龙须胶、淀粉、糊精、藻酸钠、乳糖、葡萄糖、淀粉分解物、脱脂奶粉、全乳、大豆蛋白、豆奶、植物油脂(可可脂、椰子脂等)、动物油(鱼油等)、植物提取物、甲基纤维素和羧甲基纤维素等。另外,作为这些赋形剂的物质,至少一种是用作涂布剂,把干燥的粉末包覆。通过这种包覆,所得到的醋蛋白粉变成缓慢释放性,口服时,可以缓和对粘膜的刺激性,嗜好性也可进一步改善。而且,胡罗卜素、维生素B1、维生素B2、维生素B6、维生素B12、维生素C、维生素D、维生素E、维生素K1、维生素K2和尼克酸等维生素类也可以配合。
而且,除赋形剂外,还可以配合,例如蔗糖醋酸酯、甘油脂肪酸酯、大豆卵磷脂、山梨聚糖脂肪酸酯等乳化剂等。
按照上述的本发明第一实施方案的方法所制得的醋蛋粉,可食用酸的嗅味无残留,特别是无醋酸味,然而,通过适当的焙煎,可使其具有愉快的芳香味,极富于嗜好性,优异的饮食性。
另外,按照本发明的第二实施方案,采用水解酶制得的含可溶化全蛋成分粉末,由于蛋壳钙变成水溶性,并且,蛋白和蛋黄中的蛋白质变成低分子,脂质和糖质也被分解,所以,不仅格外改善了它们的生物吸收性,而且,含有丰富的各种矿物质、维生素类、糖类、酶类、氨基酸类和有机酸类,从而,其作饮食使用也是优异的。
因此,按照本发明的方法制得的醋蛋粉,作为综合营养补品,滋养食品是极有用的。
而且,按照本发明提供的醋蛋粉,根据需要,还可以制成添加食品香料等的赋香料、甜味剂和天然色素等食品添加剂类制品,还可以制成粉状、粒状、薄片状、胶囊状以及其他所希望的食品形态。例如,将其混入或溶解在食用油(动植物油)、可可脂、棕榈油、白巧克力等中,通过成型,制成固体食品。另外,还可制成酒类及其他饮料形态,并且,还可以作为强化食品用的添加剂。
下面,通过实施例更具体地说明本发明的方法。
实施例
实施例1
往鸡的全蛋1kg里添加酿造的醋2L,于室温放置5天,蛋壳溶解时,将其破碎,用布过滤,在往滤液中吹入温度200℃、排气温度125℃的条件下进行喷雾干燥,得到了醋酸味极少,且具有来自蛋焙煎而得的理想芳香味的醋蛋粉380g。
实施例2
往鸡的全蛋1.1kg里添加5%醋酸水溶液2.5L,再添加相当于全蛋0.05%(重量)的含糖胃蛋白酶(ミクニ化学产业(株))以及0.05%(重量)的根霉菌属酶(天野制药(株)),于室温放置4天后,用搅拌器进行充分搅拌,再于室温放置1天后过滤,把滤液于80℃灭菌10分钟,再将该液于吹入温度210℃、排气温度130℃的条件下进行喷雾干燥,得到可溶化的醋蛋粉410g。
实施例3
往鹌鹑的全蛋1kg里添加酿造醋2.5L,再添加相当于全蛋0.1%(重量)的含糖胃蛋白酶(ミクニ化学产业(株))及肌酸酶(大和化成(株))0.05%(重量),于室温放置2天,蛋壳溶解时将其破碎,用布过滤,减压浓缩至滤液 1/2量,往该浓缩滤液中添加乳糖100g及脱脂奶粉200g,用吹入温度190℃、排气温度120℃进行喷雾干燥,得到可溶化的鹤鹑蛋粉700g。
实施例4
往鸡的全蛋1.1kg里添加5%醋酸水溶液2.5L,再添加相当于全蛋0.05%(重量)的含糖胃蛋白酶(ミクニ化学产业(株))及根霉菌属酶(天野制药(株))0.05%(重量),于室温放置4天后,用搅拌器充分搅拌,再放置1天后过滤,把滤液于80℃灭菌10分钟后,用吹入温度190℃、排气温度110℃进行喷雾干燥,得到可溶化的醋蛋粉430g。
实施例5
把酿造的食醋2L分别添加了3g柠檬酸及苹果酸所构成的溶液,加入鸡的全蛋1.1kg中,用搅拌器加以混合后,添加相当于全蛋0.05%(重量)的脂肪酶(天野制药(株))及胰酶制剂(天野制药(株))0.05%(重量),放置2天后,除去固体成分,把得到的分解生成物液低温减压浓缩 1/2的量,把该浓缩液在吹入温度190℃、排气温度115℃下进行喷雾干燥,得到可溶化的醋蛋粉380g。
实施例6
往鸡的全蛋1.1kg里添加酿造的食醋2.5L,用搅拌器加以混合后,添加作为酶制剂的肌酸酶(大和化成(株)),其添加量为全蛋的0.05%(重量),于35℃消化24小时后,除去固体成分,对其原封不动的用吹入温度190℃、排气温度115℃进行喷雾干燥,得到可溶化的醋蛋粉400g。
实施例7
把已添加了柠檬酸和苹果酸各3g的酿造醋3L所构成的溶液,添加至鸡全蛋1.1kg里,用搅拌器混合后,分别添加各相当于全蛋0.05%(重量)的含糖胃蛋白酶(ミクニ化学产业(株))、脂肪酶(天野制药(株))和胰酶制剂(天野制药(株)),放置2天后,除去固体成分,把所得到的分解生成物低温减压浓缩至1/2的量,把溶解明胶15g的水溶液添加至该浓缩液中,用吹入温度200℃、排气温度125℃进行喷雾干燥,得到了用明胶和藻酸包覆的可溶化醋蛋粉610g。
实施例8
往鸡的全蛋1.1kg里添加酿造醋3L,再添加蛋壳和碳酸钙以1∶1的重量比构成的混合物100g,添加作为酶制剂的肌酸酶(大和化成(株)),添加量相当于全蛋的0.5%(重量),于35℃消化24小时后,除去固体成分,添加糊精200g、胶原蛋白50g及乳糖100g,在吹入温度210℃、排气温度130℃的条件下进行喷雾干燥,得到可溶化的醋蛋粉950g。
实施例9
往1.1kg鸡的全蛋里添加酿造醋2.5L,反应4天使蛋壳溶解后,添加相当于全蛋0.02%(重量)的生物淀粉酶(天野制药(株))、0.02%(重量)的含糖胃蛋白酶(ミクニ化学产业(株))以及0.01%(重量)的胰酶制剂(天野制药(株)),于30℃消化24小时,除去固体成分,往该浓缩液中添加糊精300g及乳糖200g,在吹入温度200℃、排气温度130℃下进行喷雾干燥,得到可溶化的醋蛋粉980g。
实施例10
把实施例1或4中得到的醋蛋粉100g、乳糖50g以及糊精50g加以混合,造粒,得到200g稳定的嗜好性优异的新型醋蛋食品。
实施例11
把实施例9得到的醋蛋粉20g、橄榄油50g及作为分散剂的蜂蜡2.5g加以混合,各取300mg用常规方法填充至软胶囊中,制成胶囊食品。
实施例12
把实施例5得到的醋蛋粉,添加至面包原料中(富强粉150g、砂糖10g、酵母1.7g、食盐25g、水125g、奶油10g)使达到10%,用通常的面包制造配方及方法进行面包的制造。所得到的面包为具有特殊芳香、上等质量的含醋蛋的面包。
实施例13
将实施例1得到的含水40g的醋蛋粉5g,注入到作为饼用乳脂原料的食用油脂45g、脱脂奶粉4g以及单维生素A(チノグリ レシチン)1g中使其乳化。得到的乳化物,用高压均化机在120kg/cm2的压力下使其均化,于90℃杀菌15秒钟,制成饼用乳脂。
实施例14
把实施例6中得到的醋蛋粉3g,添加至作为冰乳脂原料的无盐奶油7g、脱脂奶粉5g、脱脂炼乳10g、生乳脂10g、蔗糖7g、CMC 0.3g以及水55.7g中,用通常的冰乳脂制造方法制造含有醋蛋的冰乳脂。
参考例1
把本发明实施例1及6中得到的醋蛋(下面分别称作本发明产物1及2)和用超细粉碎机只把鸡蛋壳加以超细粉碎,制成微细粉末(对照品1),检测钙成分的肠道吸收能力。
取试样15mg溶于15mL的生理盐水中,将其注入袋状的小鼠肠道(约20cm)中,把该肠道浸渍在生理盐水中,于37℃进行孵化,通过测定从肠道内移动到外侧生理盐水中的钙(Ca2+),试验肠道的吸收能力。其结果示于表1。
表1钙的肠道吸收比较实验
移动的钙量(μg) | ||
20分钟后 | 40分钟后 | |
本发明产物1 | 1050 | 2200 |
本发明产物2 | 1100 | 2550 |
对照产物1 | 150 | 230 |
从表1的结果可知,任何一个试样尽管用同一种鸡的蛋壳钙原料,然而,与对照品相比,通过肠道壁的吸收速度及吸收量,本发明的产品均显著优异。
Claims (10)
1.一种醋蛋粉的制造方法,其特征是,往包括蛋壳的全蛋里添加可食性酸水溶液及水解酶,于0~50℃的温度下进行分解处理,将得到的分解物生成液,根据场合,进行加热灭菌处理及/或过滤后,加以干燥,制成粉末。
2.根据权利要求1所述的方法,其中,采用喷雾干燥法使其干燥,制成粉末。
3.根据权利要求1所述的方法,其中,喷雾干燥是在吹入温度190℃~230℃、排气温度120℃~170℃的条件下进行的。
4.根据权利要求1所述的方法,其中,先往包括蛋壳的全蛋中添加可食性酸水溶液进行分解处理,在蛋壳溶解的阶段制成破碎乳液,往该乳液添加水解酶,再进行分解处理。
5.根据权利要求1所述的方法,其特征在于,把包括蛋壳的全蛋破碎,制成全蛋破碎乳液,往该乳液中添加可食性酸水溶液及水解酶,于0~50℃的温度下进行分解处理,把所得到的分解物生成液,根据场合,进行加热灭菌处理及/或过滤后,进行喷雾干燥。
6.根据权利要求1所述的方法,其中,可食性酸水溶液为米醋、黑醋、苹果醋、醋酸水溶液、苹果酸水溶液、柠檬酸水溶液、琥珀酸水溶液、乳酸水溶液或它们的混合物。
7.根据权利要求1所述的方法,其中,水解酶为选自肌酸酶、生物淀粉酶、根霉菌属酶、脂肪酶、卵磷脂酶、胰酶制剂和胃蛋白酶的水解酶制剂。
8.根据权利要求1所述的方法,其中,在制造的任意阶段,以选自蛋壳粉、碳酸钙、醋酸钙和乳酸钙钙源作为钙,并以每100g原料蛋为1~10g的比例添加。
9.根据权利要求1所述的方法,其中,所得到的醋蛋粉,再用可食性的涂布剂加以包覆。
10.配合按照权利要求1所述的方法得到的醋蛋粉的食品。
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1999
- 1999-09-17 AU AU56526/99A patent/AU768268B2/en not_active Ceased
- 1999-09-17 EP EP99943381A patent/EP1050220A4/en not_active Withdrawn
- 1999-09-17 KR KR10-2000-7004814A patent/KR100500004B1/ko not_active IP Right Cessation
- 1999-09-17 WO PCT/JP1999/005068 patent/WO2000018257A1/ja active IP Right Grant
- 1999-09-17 CN CNB998016594A patent/CN1165245C/zh not_active Expired - Fee Related
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WO2000018257A1 (fr) | 2000-04-06 |
CN1286595A (zh) | 2001-03-07 |
EP1050220A1 (en) | 2000-11-08 |
KR20010031749A (ko) | 2001-04-16 |
EP1050220A4 (en) | 2004-06-02 |
KR100500004B1 (ko) | 2005-07-12 |
TW575403B (en) | 2004-02-11 |
AU5652699A (en) | 2000-04-17 |
JP4221637B2 (ja) | 2009-02-12 |
HK1034165A1 (en) | 2002-09-27 |
AU768268B2 (en) | 2003-12-04 |
CA2311527A1 (en) | 2000-04-06 |
US6358554B1 (en) | 2002-03-19 |
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