CN1433304A - 睡眠促进用组合物 - Google Patents
睡眠促进用组合物 Download PDFInfo
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- CN1433304A CN1433304A CN01810707A CN01810707A CN1433304A CN 1433304 A CN1433304 A CN 1433304A CN 01810707 A CN01810707 A CN 01810707A CN 01810707 A CN01810707 A CN 01810707A CN 1433304 A CN1433304 A CN 1433304A
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Abstract
本发明的目的是提供不必担心副作用、日常中任何人都能够放心使用的、含有茶氨酸的睡眠促进用组合物。此外，本发明的目的是提供对睡眠障碍个体适用的、具有睡眠促进效果的含有上述组合物的食品或者医药用品。并且，本发明的目的是提供将茶氨酸用药于睡眠障碍个体的睡眠促进方法，以及提供用于制造适用于睡眠障碍个体的食品或者医药用品的茶氨酸的使用。
Description
技术领域
本发明涉及含有茶氨酸的睡眠促进用组合物、含有该组合物的食品或者药品、利用茶氨酸促进睡眠的方法，以及用于制造上述食品或者医药用品的茶氨酸的使用。
背景技术
睡眠障碍是可能导致酒精依赖症、睡眠药物等的药物依赖症、麻药中毒等的前期障碍，如何克服睡眠障碍和防止这类问题很有社会意义。目前，针对这类睡眠障碍采用三唑仑或者布酰胺等治疗性药品，不过这类药品存在眩晕和健忘以及依赖性情绪不稳定等人们不期望出现的副作用，并且无医生指导时服用会很危险，而且还具有并不是所有睡眠障碍者都可以服用的缺点。总之，当前的现状是以前合成的药品存在发生副作用的缺点，而有效的治疗方法尚未发现。
发明的内容
本发明的目的是提供不必担心副作用、日常中任何人都能够放心使用的睡眠促进用组合物。此外，本发明的目的是提供对睡眠障碍个体适用的具有睡眠促进效果的食品或者医药用品。并且，本发明的目的是提供用于睡眠障碍个体的有效的睡眠促进方法，以及提供用于制造适用于睡眠障碍个体的上述食品或者医药用品的茶氨酸的使用。
为了解决上述课题，本发明者等人不断重复刻苦钻研，结果发现茶氨酸能够有效地促进睡眠，并且不伴有发生副作用的问题，完成了本发明。
即，本发明涉及，
〔1〕睡眠促进组合物，其特征在于含有茶氨酸、
〔2〕含有上述〔1〕记载的组合物、适用于睡眠障碍个体的食品、
〔3〕含有上述〔1〕记载的组合物、适用于睡眠障碍个体的药品、
〔4〕将茶氨酸施用于睡眠障碍个体的睡眠促进方法、以及
〔5〕用于制造适用于睡眠障碍个体的食品或者药品的茶氨酸的使用。实施发明的最佳状态
本发明的睡眠促进用组合物(以下称为组合物)能够在日常生活中使用，以缓和或者改善由各种原因导致产生的各种睡眠障碍。本发明的组合物发挥预期效果是基于组合物中所含茶氨酸的首次被发现的睡眠促进作用。
本发明所用的茶氨酸是谷氨酸的衍生物(γ-glutamylethylamide)，是天然茶叶中富含的氨基酸成分。在本发明中发现的茶氨酸的睡眠促进作用的作用机理尚且有很多不清楚的地方，不过已知在组成睡眠的6个阶段StageW、Stage1、Stage2、Stage3、Stage4和StageREM中在睡眠导入阶段StageW中α波所占的比例在50％以上，之后，Stage1中发生脑波变化，即α波减少、δ波增加，推测茶氨酸对于脑波的变化会产生某些影响引发了上述作用的发挥。即，在本发明书中的“促进睡眠”指的是保持生物体睡眠的恒定性，促进自然睡眠的进行。并且，本发明的组合物不必担心发生依赖症等副作用，能够如愿地在日常生活中使用。例如使用含有茶氨酸的本发明组合物，可以缓和或者改善例如由于生物体节律失调导致的各种睡眠障碍(例如失眠症、难眠(入睡困难)、睡眠中途醒来、清晨过早醒来、熟睡障碍等)。
并且，本发明所用的茶氨酸的睡眠促进作用的发挥，可以通过多道记录仪测量睡眠导入阶段的脑波的变化进行判断。即，当发现上述睡眠导入阶段的脑波变化时，确认进入睡眠状态。比较茶氨酸的施用个体和非施用个体进入睡眠状态的时间，发现茶氨酸施用个体比非施用个体更早进入睡眠状态，由此确定茶氨酸具有睡眠促进作用。此外，如果使用多道记录仪不仅能够观察记录脑波，还可以同时观察记录心电图、眼球运动、肌电图、呼吸曲线等生体现象，根据这些脑波以外的项目也能够确定茶氨酸具有睡眠促进作用。
作为本发明所用的茶氨酸的制造方法，例如，从茶叶中抽提的方法、有机合成法〔Chem.Pharm.Bull.，19(7)1301-1307(1971)〕、将谷氨酰胺和乙胺的混合物经谷酰胺酶作用的方法(特公平第7-55154号公报)、在含有乙胺的培养基中培养茶的培养细胞群，一边增加培养细胞群中的茶氨酸的蓄积量一边使培养细胞群的增殖促进的方法(植物细胞培养法)(特开平第5-123166号公报)、此外，特开平第7-55154号公报、特开平第5-123166号公报中，将上述植物细胞培养法中的乙胺置换成乙胺盐酸盐等乙胺衍生物的改进方法等任何众所周知的方法都可以。此外，所用的茶氨酸的形态可以是纯化品、粗纯化品、抽提浸膏等任何形态。并且，此处所说的茶叶，可以举出绿茶茶叶、乌龙茶茶叶、红茶茶叶等。也可以使用市售商品〔SUNTHEANINE(注册商标)太阳化学(股份)公司制造〕。
茶氨酸可以使用L-茶氨酸，D-茶氨酸，DL-茶氨酸中的任何一种，其中，因为L-茶氨酸许可作为食品添加剂，而且在经济上可以便宜利用，所以本发明优选L-体。
在本发明的组合物中的茶氨酸的含量没有特殊的限制，只要根据所需适当调整即可。例如，组合物中的适当的茶氨酸的含量优选5～100重量％，尤其优选50～100重量％。
本发明的组合物可以另外含有各种矿物质。含有矿物质的组合物，尤其优选能够发挥补充生物体内容易不足的必需元素、微量必需元素的效果的组合物。组合物中的矿物质的含量优选例如0.0001～99.9重量％、更优选0.01～99.9重量％。该矿物质可以举出铁、镁、铜、锌、硒、钙、钾、锰、铬、碘、钼、镍、钒等维持、调节生物体的稳定性的必须的金属类或这些金属的盐类。这些物质可以单独使用或者两种以上混合使用。
此外，同时含有天然药物、草药、氨基酸、维生素等亦可。所包括的天然药物没有特殊的限制，优选对稳定精神有效的灵芝、地黄茎、大枣等。此外，草药没有特殊的限制，例如，茴香、胡萝卜籽、丁香、胡荽、柏木、桂皮、杜松、生姜、甜橙、松针、罗勒、绿叶刺蕊草、苦橙、小茴香、黑胡椒、月桂、薄荷、香柠檬、蜜桔、没药、柠檬香茅、迷迭香、葡萄柚、香柏木、香茅、鼠尾草、麝香草、茶树、紫叶、香草、海索草、桉树、石灰、柠檬、衣兰、小豆蔻、鼠尾草、茉莉、天竺葵、甘菊、保加利亚玫瑰、玫瑰、乳香、薰衣草、甘菊、檀香、橙花油、马鞭草、橙叶(プチグレン)、岩兰草、牛至、柠檬香脂(メリッサ)、玫瑰木、金丝桃、圣.约翰麦芽和鲔，其中优选有镇静和放松效果的薄荷、香柠檬、衣兰、天竺葵、甘菊、薰衣草、圣.约翰麦芽和鲔。这些草药的形态例如可以是抽提浸膏、精油、草药茶等，没有特殊的限制。氨基酸也没有特殊的限制，例如可以是：谷氨酰胺、谷氨酸、色氨酸、丙氨酸、精氨酸、天冬氨酸、苏氨酸、丝氨酸、γ-氨基丁酸、氨基乙磺酸、硫代牛磺酸和亚牛磺酸。维生素没有特殊限制，例如有，维生素A、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K、叶酸、烟酸、硫辛酸、泛酸、生物素、辅酶Q和前列腺素以及这些维生素的衍生物。此外，其他的成分有，例如，芦荟、蜂王浆、褪黑激素、胎盘、蜂胶、异黄酮、大豆卵磷脂、蛋黄卵磷脂、蛋黄油、软骨素、可可块、胶原、醋、小球藻、螺旋藻属(スピルリナ)、银杏叶、绿茶、杜仲茶、黄妃茶、乌龙茶、桑叶、甜茶、大花紫薇(バナバ)茶、不饱和脂肪酸、寡糖等糖类；双歧杆菌和日本清酒曲等菌类；伞菌属、姬マッタケ、マィタケ等蘑菇类；越橘、干梅子、葡萄、橄榄、日本杏和柑橘等水果；花生、杏仁、芝麻和辣椒等种子；绿辣椒、红辣椒、威尔士洋葱、南瓜、葫芦、胡萝卜、牛蒡、黄麻叶、蒜、紫苏、山萮菜、西红柿、韭葱、蔬菜叶、块茎和豆子等蔬菜；裙带菜等海草类；鱼类；兽、鸟、鲸肉类；谷类等，可以根据需要适当的选择使用这些物质或者这些物质的抽提物、干燥品、粗纯化品、纯化品、加工品、酿造品等。
此外，作为本发明的一种状态，提供含有本发明组合物的、适合日常使用的、适用于睡眠障碍个体的食品或者药品。这种食品或者药品只要是含有茶氨酸的组合物即可，没有特殊限制。并且，在本发明书中的“个体”例如以哺乳动物为例，具体指人、猪、牛、狗、猫和马等，特别优选人。
作为本发明的食品，含有茶氨酸，可以举出以下例示的各种食品。
这些食品例如可以举出固态食品，以及清凉饮料和矿泉水、高级饮品、酒精饮料等液态食品。这里列举的液态食品并无特殊的限制，优选绿茶、乌龙茶、红茶、药草茶等茶类，浓缩果汁、浓缩还原果汁、纯鲜果汁、复合水果果汁、加入果肉的水果果汁、加入果汁的饮料、水果-蔬菜复合汁、蔬菜汁、矿泉水、碳酸饮料、清凉饮料、牛奶、乳品饮料、日本酒、啤酒、葡萄酒、鸡尾酒、烧酒、威士忌等。此外，固态食品也没有特殊限制，优选酱制品、大豆加工品、驼鹿(ム-ス)、胶冻、乳酸、冷点、糖、巧克力、口香糖、薄脆饼干、小点心、曲奇饼干、面包等。
此外，本发明的药品只要是含有茶氨酸的即可，没有特殊限制。例如其形态可以是溶液、悬浊物、粉末、固体成型物等中的任何一种，其剂型可以举出片剂、胶囊、粉末、颗粒、饮料剂等。此外，还可以和其他药品合并使用。
并且，上述本发明的食品或者药品，也可以以人以外的个体为对象，例如，可以用于有睡眠障碍的哺乳动物，例如可以根据需要制成用于牛、猪、马等家畜和狗、猫宠物等的具有睡眠促进效果的饲料、饮料、制剂、试剂等。
本发明的组合物的制备方法没有特殊的限制，例如可以使用，将茶氨酸和其他的原材料进行粉混合的制备法、将茶氨酸和其他的原材料融解于溶剂中制成混合溶液的制备法、还有将这种混合溶液冻干的制备法、喷雾干燥制备法等使用于普通食品或者药品的制备法。本发明的食品或者药品都同样适用。此外，能用于制造本发明的组合物中除了茶氨酸之外的成分，只要不阻碍茶氨酸的效果的发挥，可以根据所希望的用途进行适当的选择。
例如，对于现存的食品，制造后的本发明食品中茶氨酸的含量优选在上述组合物中的适宜的茶氨酸含量范围内，按照常规方法配入茶氨酸进行本发明食品的制造。此外，和食品制造时一样，将茶氨酸和例如众所周知的与经口施用相适宜的有机或者无机的载体、赋形剂、结合剂、稳定剂等，优选在上述适宜的茶氨酸的含量范围内，将茶氨酸按照常规方法配入进行药品的制造。在制造所述本发明的睡眠障碍个体适用的食品或者药品时的茶氨酸的使用也包括在本发明范围内。
并且，作为本发明的一种形式，提供将茶氨酸施用于睡眠障碍个体的睡眠促进方法。如果采用此方法，不用担心发生副作用，能够安全、有效的促进该个体的睡眠，进而能够有效地缓和或者改善该个体的睡眠障碍。在本形式中，为了达到本发明所预期的效果，茶氨酸的有效施用量，一般情况下，例如：针对人时，成人优选每天0.2～200mg/kg体重，更优选0.5～50mg/kg体重。当然，由于存在不同个体的睡眠障碍的种类、程度和个体差异(年龄、性别等)，本发明的茶氨酸的使用量并不只限于所述范围。
施用茶氨酸，可直接使用茶氨酸或者也可以使用本发明的组合物，优选使用食品或者药品。此外，施用方法、施用次数、施用时间等没有特殊的限定。上述个体优选针对希望缓解或改善睡眠障碍的人，例如分成一次或者数次，优选经口施用，以在上述有效施用量范围内施用为好。可以通过日常性地摄取茶氨酸或本发明的组合物等预防睡眠障碍。
在本发明中使用的茶氨酸的安全性高，例如进行鼠的急性毒性试验时，在5g/kg经口施用时没有发生死亡，也没有发生一般状态以及体重等的异常。此外，尤其是已知L-茶氨酸作为茶风味的主要成分用于呈现风味用途的食品添加剂，在食品卫生法上，其添加量没有限制。并且，与一贯的睡眠障碍改善药物不同，完全没有检测到茶氨酸的依赖性，因此本发明的组合物、食品或者药品能够安全并且有效的促进睡眠，能够缓和或改善睡眠障碍。
实施例
下面通过实施例对本发明进行更详细的说明，不过本发明的范围并不仅限于这些实施例。并且，在实施例中“份”没有其他意思，只表示“重量份”。制造例1
0.3M谷氨酰胺和1.5M乙胺在硼酸缓冲液(Na2B4O7-NaOH，pH＝11)中与0.3U谷酰胺酶(天野制药(股份)公司制造)在30℃，反应22个小时。然后，将反应液上样到使用Dowex 50×8和Dowex 1×2(均由市町化学工业(股份)公司制备)的色谱柱上，用乙醇进行处理，从反应液中分离目的物质。
判定此物质为L-茶氨酸是通过将得到的分离物进行氨基酸分析和纸层析，根据此物质和标准物质产生一样的行为进而判定的。当用盐酸或者谷酰胺酶进行水解处理时，此物质能够按照1∶1(摩尔比)的比例生成谷氨酸和乙胺。这样一来，分离物质的谷酰胺酶水解反应表示乙胺结合在谷氨酸的γ位。此外，水解反应生成的谷氨酸是L-构型体也可以通过谷氨酸脱氢酶进行确认，由此确定所得到的分离物是L-茶氨酸。
根据以上操作，得到225nmol的L-茶氨酸。并且，得到20nmol副产物谷氨酸。制造例2
将茶(Camellia sinensis L.)叶10kg用热水进行抽提后，通过阳离子交换树脂(市町化学工业(股份)公司制造，Dowex HCR W-2)用1N NaOH进行溶出。将溶出组分通过活性炭(二村化学工业(股份)公司制备，太阁活性炭SG)后，将用15％的乙醇溶出的组分利用RO膜(日东电工(股份)公司制造，NTR 729HF)进行浓缩，在色谱柱进行纯化，进一步进行再结晶，得到L-茶氨酸24.8g。
实施例1
将制造例1中得到的L-茶氨酸按照下面的配方制造含有茶氨酸的糖果。
含有茶氨酸的糖果
1.砂糖 64份
2.麦芽糖浆 23份
3.L-茶氨酸 10份
4.香料(柠檬香料) 0.05份
5.酒石酸 1份
6.水 30份
将砂糖完全溶解在20份水中，同时加热到110℃，加入麦芽糖浆，使温度上升直到145℃。止火，添加酒石酸混合后，添加事先溶解了L-茶氨酸的剩余的水。再次混合，冷却到75～80℃，用成形辊进行成形，得到每粒1g的糖果。
实施例2
将制造例2中得到的L-茶氨酸按照下面的配方制造含有茶氨酸的胶囊。
含有茶氨酸的胶囊
1.L-茶氨酸(太阳化学(股份)公司制造) 98份
2.阿拉伯树胶(五协产业(股份)公司制造) 2份按照常规方法，将L-茶氨酸的粉末包入阿拉伯树胶中，得到含有茶氨酸的胶囊。
实施例3
将实施例1制造的糖果给5名苦于就寝无法入睡的患者(躺在床上后在1个小时以上不到1.5个小时的时间范围内不能够入睡的人)服用，在上床30分钟前服用1粒，服用4天，有2名难以入眠者的症状得到改善，12天时，所有难以入眠者都得到改善(上床后，能在大约20分钟时间内入睡)。并且，没有发现任何不理想的副作用。
并且，在进行该试验的半个月之前，使用乳糖替代含茶氨酸的胶囊中的茶氨酸作成胶囊(对照)进行同样的试验，难以入眠的状况没有得到任何改善。
实施例4
将在实施例2中得到的含有茶氨酸的胶囊(L-茶氨酸：200mg/个)给诊断患有失眠症的3名患者(上床后经过1.5小时以上还不能入睡的人)服用，在上床前30分钟服用1粒，当服用4天时，3名患者的失眠症都得到解除(上床后在20分钟以内能入睡)。并且，没有发现任何不理想的副作用。
并且，在进行该试验的半个月之前，使用乳糖替代茶氨酸的胶囊中的茶氨酸制成胶囊(对照)进行同样的试验，失眠症的状况没有得到解除。
产业上利用的可能性
根据本发明，提供不必担心副作用的、任何人都能够在日常中放心使用的睡眠促进组合物。此外，根据本发明，提供具有适用于睡眠障碍个体的具有睡眠促进效果的食品或者药品。并且，根据本发明，提供将茶氨酸施用给睡眠障碍个体的睡眠促进方法。
Claims (5)
1.睡眠促进用组合物，其特征在于含有茶氨酸。
2.食品，其中含有权利要求1所述的组合物，适用于睡眠障碍个体。
3.药品，其中含有权利要求1所述的组合物，适用于睡眠障碍个体。
4.睡眠促进方法，其中，将茶氨酸施用于睡眠障碍个体。
5.茶氨酸的使用，其用于制造适用于睡眠障碍个体的食品或者药品。
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| CA (1) | CA2404387C (zh) |
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| WO (1) | WO2001074352A1 (zh) |
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| CN103461589A (zh) * | 2013-09-06 | 2013-12-25 | 北京绿源求证科技发展有限责任公司 | 一种改善睡眠的食品助眠茶冲剂 |
| CN106135909A (zh) * | 2015-06-06 | 2016-11-23 | 重庆两江药物研发中心有限公司 | 一种食品组合物及其制备方法和用途 |
| WO2018058984A1 (zh) * | 2016-09-30 | 2018-04-05 | 深圳市贝沃德克生物技术研究院有限公司 | 基于健康促进的适合失眠人群饮用的饮品及其制备方法 |
| CN111617013A (zh) * | 2020-07-23 | 2020-09-04 | 泉后(广州)生物科技研究院有限公司 | 一种具有助眠功效的组合物、喷雾及其制备方法 |
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| JP4961087B2 (ja) * | 2000-04-05 | 2012-06-27 | 太陽化学株式会社 | 睡眠促進用組成物 |
| JP4824152B2 (ja) * | 2000-04-28 | 2011-11-30 | 太陽化学株式会社 | 血流改善剤 |
| DE10035190C5 (de) | 2000-07-20 | 2009-07-16 | MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. | Verfahren und Vorrichtung zur Fluoreszenzmessung |
| JP3730522B2 (ja) * | 2000-07-21 | 2006-01-05 | 太陽化学株式会社 | 喫煙欲求抑制組成物 |
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| EP3662919A1 (en) | 2015-08-31 | 2020-06-10 | Nutramax Laboratories, Inc. | Compositions comprising magnolia, phellodendron, theanine and/or whey protein |
| KR101685631B1 (ko) * | 2016-06-10 | 2016-12-13 | 순천대학교 산학협력단 | 숙면용 한방 방향제 |
| JP6873291B1 (ja) | 2020-02-05 | 2021-05-19 | 雪印メグミルク株式会社 | 睡眠促進用組成物及び組成物を含む食品、医薬品、飼料 |
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| JPH0755154B2 (ja) | 1991-09-14 | 1995-06-14 | 太陽化学株式会社 | テアニンの製造方法 |
| JPH05123166A (ja) | 1991-10-31 | 1993-05-21 | Food Design Gijutsu Kenkyu Kumiai | 茶の培養細胞群の増殖法 |
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| AU1525695A (en) * | 1994-01-10 | 1995-08-01 | Procter & Gamble Company, The | Tea extract and process for preparing |
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| US6271259B1 (en) * | 1996-05-07 | 2001-08-07 | Ito En, Ltd. | Method for improving the brain function, inhibiting glutamate excitotoxicity and rescuing from neuronal death |
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| JP4961087B2 (ja) * | 2000-04-05 | 2012-06-27 | 太陽化学株式会社 | 睡眠促進用組成物 |
| US20020122835A1 (en) * | 2001-03-01 | 2002-09-05 | Bucci Luke R. | Compositions for enhancing muscle tissue recovery and repair |
| CA2500417A1 (en) * | 2002-10-15 | 2004-04-29 | Shoei Furukawa | Neurotrophic factor production promoter |
| US20050191341A1 (en) * | 2004-03-01 | 2005-09-01 | Gottfried Kellermann | Liposomal composition comprising L-theanine |
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2001
- 2001-04-04 JP JP2001572097A patent/JP4961087B2/ja not_active Expired - Lifetime
- 2001-04-04 WO PCT/JP2001/002916 patent/WO2001074352A1/ja active IP Right Grant
- 2001-04-04 US US09/980,620 patent/US7273621B2/en not_active Expired - Lifetime
- 2001-04-04 KR KR1020027013274A patent/KR20020089430A/ko not_active Application Discontinuation
- 2001-04-04 MX MXPA02009794A patent/MXPA02009794A/es not_active Application Discontinuation
- 2001-04-04 EP EP01921790A patent/EP1277468A4/en not_active Withdrawn
- 2001-04-04 AU AU4874201A patent/AU4874201A/xx active Pending
- 2001-04-04 AU AU2001248742A patent/AU2001248742B2/en not_active Ceased
- 2001-04-04 CA CA2404387A patent/CA2404387C/en not_active Expired - Lifetime
- 2001-04-04 CN CNB018107079A patent/CN100374108C/zh not_active Expired - Lifetime
-
2007
- 2007-08-23 US US11/843,913 patent/US8293269B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103461589A (zh) * | 2013-09-06 | 2013-12-25 | 北京绿源求证科技发展有限责任公司 | 一种改善睡眠的食品助眠茶冲剂 |
| CN106135909A (zh) * | 2015-06-06 | 2016-11-23 | 重庆两江药物研发中心有限公司 | 一种食品组合物及其制备方法和用途 |
| WO2018058984A1 (zh) * | 2016-09-30 | 2018-04-05 | 深圳市贝沃德克生物技术研究院有限公司 | 基于健康促进的适合失眠人群饮用的饮品及其制备方法 |
| CN111617013A (zh) * | 2020-07-23 | 2020-09-04 | 泉后(广州)生物科技研究院有限公司 | 一种具有助眠功效的组合物、喷雾及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4961087B2 (ja) | 2012-06-27 |
| US20020188025A1 (en) | 2002-12-12 |
| EP1277468A1 (en) | 2003-01-22 |
| CA2404387A1 (en) | 2001-10-11 |
| EP1277468A4 (en) | 2003-06-11 |
| WO2001074352A1 (fr) | 2001-10-11 |
| US7273621B2 (en) | 2007-09-25 |
| CN100374108C (zh) | 2008-03-12 |
| AU2001248742B2 (en) | 2005-07-14 |
| MXPA02009794A (es) | 2004-06-14 |
| US20080039526A1 (en) | 2008-02-14 |
| AU4874201A (en) | 2001-10-15 |
| KR20020089430A (ko) | 2002-11-29 |
| US8293269B2 (en) | 2012-10-23 |
| CA2404387C (en) | 2011-01-11 |
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