CN109070130B - 用于标记纤维素产品的方法 - Google Patents
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Abstract
用于标记纤维素产品的方法,该纤维素产品包括诸如莱赛尔纤维(lyocell)和纤维素膜的纤维素纤维,该方法包括利用可检测的核酸标记物标记此类产品以识别和验证产品或使用此类产品制造的物品的来源或真实性的方法。还提供了用于认证、验证和跟踪的利用核酸标记物标记的可检测标记的纤维素产品。
Description
相关申请的引证
本申请要求2016年4月11日提交的美国专利临时序列号62/320,946的优先权,在此通过引证将其并入到本申请中。
技术领域
本发明涉及用于标记纤维素产品(产物,product)的方法,该纤维素产品包括莱赛尔纤维(木浆纤维,lyocell)和纤维素膜,并且更具体地涉及利用核酸标记物标记此类产品以识别和验证产品或使用此类产品制造的物品的来源或真实性的方法。
背景技术
制造商有兴趣保护其产品的完整性和纯度,这些产品由优质组件制成,并且可以经受利用较便宜、质量较低的材料进行混合或稀释。来自供应商的由制造商加工的这种掺假甚至是彻底的假冒替代工艺原料和生产材料,往往在产品制造之后就无法检测到。
高端产品的假冒特别是与更便宜的材料的共混,已成为许多公司的主要责任问题。国际商会(ICC)报告称,2008年,假冒商品造成了6500亿美元的收入损失和250万个就业岗位的损失。国际商会预计2015年的收入损失将超过1.7万亿美元,相当于世界经济的2%。除收入损失外,各种假冒产品还涉及严重的健康和安全问题。
发明内容
在一个实施方式中,本发明提供了一种标记纤维素产品用于认证的方法:该方法包括在用于生产纤维素产品的工艺的一个步骤期间将可检测的核酸标记物添加到纤维素介质中;以及从而将所述可检测的核酸标记物掺入至所述纤维素产品中,以提供可检测标记的纤维素产品。优选的纤维素产品是莱赛尔纤维。
在另一个实施方式中,本发明提供了一种认证纤维素产品的方法:该方法包括:在用于生产纤维素产品的工艺的一个步骤期间将可检测的核酸标记物添加到纤维素介质中;从而将该核酸标记物掺入至纤维素产品中以提供包含核酸标记物的可检测标记的纤维素产品;将可检测标记的纤维素产品引入至商业流中;在可检测标记的纤维素产品的纤维素介质中,检测该核酸标记物的存在;以及从而认证该纤维素产品。
本发明进一步提供了一种用于认证的可检测标记的纤维素产品,其包含纤维素介质,该纤维素介质包括掺入至纤维素介质和/或在纤维素产品的纤维素介质表面上的可检测的核酸标记物。
附图说明
图1示出了由纤维素材料生产纤维素纤维或膜的工艺的步骤的示意图。
图2示出了由木屑(wood chips)、植物体(plant matter)或其他纤维素材料生产纤维素纤维或膜的工艺。紧接着在纺纱以产生纤维素纤维之前,示出了在纤维素介质中添加标记物DNA的步骤的一个实例。
图3示出了制造莱赛尔纤维,纤维素纤维,的工艺。
具体实施方式
本文所用术语的定义:
如在本文中所用的“纤维素产品”是指纤维素纤维,诸如例如粘胶纤维(viscose)、莱赛尔纤维或人造丝纤维(rayon);和纤维素膜、纸、纤维素多孔过滤器和纤维素弹性海绵。
如在本文中所用的“可检测的核酸标记物”是指任何至少部分地包括可通过许多众所周知的检测技术中的任一种检测的独特的(唯一的,unique)序列的核酸,该检测技术包括聚合酶链式反应(PCR)技术、其他DNA扩增方法诸如等温、杂交技术和任何众所周知的DNA测序方法。
如在本文中所用的“可检测的标记物DNA”是指任何至少部分地包括可通过许多众所周知的检测技术中的任一种检测的唯一的序列的DNA,该检测技术包括聚合酶链式反应(PCR)技术、其他DNA扩增方法诸如等温、杂交技术和任何众所周知的DNA测序方法。
如在本文中所用的“具有唯一的序列的核酸标记物”是指具有由所有分子共有的一致的核苷酸序列的一种或多种分子的核酸。
如在本文所用的“编码与产品相关的信息的核酸标记物”是指具有指定的核苷酸序列的核酸标记物,该指定的核苷酸序列与一种或多种与特定产品相关的数据段相关联。这种产品相关的信息和指定的核酸标记物的核苷酸序列可以存储在数据库中。该数据库用于基于指定的核酸标记物的特定核苷酸序列的检测检索产品相关的信息,从而允许认证或验证从特定产品中获得核酸标记物。核酸标记物可以在运输过程中的任何阶段或在商业流中取样,以认证或验证标记有核酸标记物的产品的完整性,该核酸标记物具有指定为与真实产品相关的核苷酸序列。
如在本文所用的“纤维素材料”包括植物体(棉花、大麻、竹子和几乎任何植物纤维素材料,以及来自山毛榉、桉树和其他树木的木屑)。这些纤维素材料可以被加工成各种不同的纤维素产品。纤维素材料通常与溶剂混合以制造纤维素产品。
“纤维素介质”可以指包括纤维素的任何介质,包括但不限于纤维素涂料(dope)。纤维素介质可以包括来自一种或多种纤维素材料的纤维素。该纤维素介质可以是浆料或液体浴,其中结合纤维素纸浆和其他化学品。
粘胶人造丝(viscose rayon)是由纤维素和黄原酸纤维素组成的半合成纤维素材料。它是一种柔软的纤维,常用于织物和服装、衬里、衬衫、短裤、外套、夹克和其他外套中。粘胶还用于工业纱线,诸如轮胎制造中结合的帘线(cords)、室内装潢(upholstery)和地毯,以及用于铸造玻璃纸膜。
人造丝纤维由再生纤维素形成,并且由于通过改变生产工艺可获得的多种特性而可以被设计成满足许多不同的需求。实例包括高湿模量人造丝纱线、超吸收人造丝和高度拉伸的低保水人造丝纤维。
纤维素产品还包括莱赛尔纤维(lyocell),另一种形式的人造丝和再造棉制品。莱赛尔纤维是一种由漂白木浆制成的纤维素人造丝产品,并且用于制作用于服装的织物和其他用途。玻璃纸是一种透明的包裹物,形成为纤维素薄膜而不是被纺成纤维。
在一个优选的实施方式中,本发明涉及通过在纤维制造工艺的预纺纱阶段期间将可检测的标记物DNA掺入莱赛尔纤维素介质中而将可检测的标记物DNA掺入莱赛尔纤维素纤维的方法。
示意性的工艺步骤
参照图1,是纤维素产品制造步骤的示意图,包括用苛性钠溶液处理纤维素浆料;将经过碱处理的纤维素材料压制成蓬松的碎屑;纤维素材料在受控的温度下老化一段时间;冷却步骤;“黄原酸化”加工步骤,使用二硫化碳(CS2)处理并溶解在碱液中并将黄色碎屑溶解在苛性钠中;过滤步骤;熟化步骤,其中使纤维素材料成熟;脱气步骤;预纺纱步骤(此时可以添加可检测的标记物核酸);洗涤步骤;拉伸步骤,然后切割并再次洗涤纤维素产品;以及干燥和打包成纤维素产品包,用于分发或运送给下游制造商。
参照图2,是用于生产纤维素产品的示例性工艺的图示,示出了在纤维纺纱之前添加DNA标记物。
参照图3,是莱赛尔纤维制造步骤的示意图。该工艺首先将木浆、水和氧化胺混合在一起以产生称为纤维素涂料的纤维素介质(优选的氧化胺是N-甲基吗啉氧化物(NMMO))。木浆溶解在作为1-1摩尔的NMMO与水的络合物的溶剂中,加热并置于加压容器中。过滤溶液。此时,可以将可检测的核酸标记物添加到纤维素涂料中。然后,使用干喷射湿纺纱工艺将纤维素涂料泵送通过喷丝头。在纺纱工艺之后,用水洗涤纤维并干燥,然后可以将润滑剂施加到纤维上。氧化胺溶剂可以从纤维工艺中回收并在制造过程中重复使用。
在一个实施方式中,本发明提供了一种标记纤维素产品用于认证的方法:该方法包括在用于生产纤维素产品的工艺的一个步骤期间将可检测的标记物诸如例如并且不限制于可检测的核酸添加到纤维素介质中;以及从而将该可检测的标记物掺入和/或嵌入纤维素产品中,以提供可检测标记的纤维素产品。在生产纤维素产品中的步骤可以是或可以不是在碱性条件下加工纤维素材料的步骤。
在一个实施方式中,本发明提供了一种标记纤维素产品用于认证的方法,包括:在纺纱或成膜纤维素产品之前或期间将可检测的核酸标记物添加到纤维素介质中,以及从而将该可检测的核酸标记物掺入纤维素产品中,以提供可检测标记的纤维素产品。
通过上面列出的方法生产出的可检测标记的纤维素产品可以是任何纤维素纤维或纤维素膜。
核酸,尤其是脱氧核糖核酸(DNA)非常适合用作使用现代方法诸如等温扩增、聚合酶链反应(PCR)和杂交检测便于检测的可检测的标记物。此外,由于DNA和RNA寡核苷酸的巨大编码能力,核酸非常适合于编码信息。可以容易地编码在核酸可检测标记物中的有用信息包括例如但不限于:生产批号、制造或加工的日期、时间以及制造商的身份。
核酸标记物
核酸非常特别适合于充当可检测的标记物,由于核酸具有巨大的编码能力,并且它们能够以如此微小的量使用的事实,使得在不知道其核苷酸序列或没有获得互补探针或其扩增所需的特定引物序列情况下无法对其进行扩增,故对其进行检测。
可检测的核酸标记物优选直接附着在纤维素纤维或薄膜上或直接嵌入纤维素纤维或薄膜中。在制造莱赛尔纤维的工艺中,核酸标记物在加入纤维素介质之前不应与任何其他“体”附着,因为在制备工艺期间添加大的“体”将会降低末端莱赛尔纤维的内部结构,莱赛尔纤维的宽度通常小于300nm。事实上,在该工艺中仅使用痕量(非常小量)的可检测的标记物DNA以确保内部纤维结构的均匀尺寸和密度不受损害。
用于掺入根据本发明的纤维素材料中的可检测的标记物DNA的合适量的范围可以从每千克纤维素材料(103g)0.1纳克(10-10g)至微克(10-6g)可检测的标记物DNA,每千克纤维素材料加入可检测的标记物DNA的优选范围为0.1纳克(10-10g)至10微克(10x10-6g)。可以仔细计量在纤维素材料加工期间添加的可检测的标记物DNA的量,用于最佳地递送合适量的DNA用于认证、验证和跟踪,还确保精细得到的纤维素产品的结构完整性。
例如,在制造莱赛尔纤维的方法中添加的可检测的标记物DNA的量的范围可以从每千克纤维素材料微克(10-6g)至小于纳克(10-9g)。在一个优选的实施方式中,在制造莱赛尔纤维的方法中添加至纤维素介质的可检测的标记物DNA的量的范围可以从每千克纤维素材料0.1纳克(10-10g)至10微克(10×10-6g)。在另一个实施方式中,可检测的标记物DNA的量小于1ppt(10-12)w/w的纤维素材料。
纤维素介质所负载的可检测的标记物DNA的合适的示例性范围包括例如:
每千克纤维素材料(10g)添加从约0.1纳克(10-10g)至约10微克(l0x10-6g)的可检测的标记物DNA的范围。
每千克纤维素材料(10g)添加从约0.1纳克(10x10-10g)至约1微克(10-6g)的可检测的标记物DNA的范围。
每千克纤维素材料(10g)添加从约0.1纳克(10x10-10g)至约100纳克(100x10-9g)的可检测的标记物DNA的范围。
每千克纤维素材料(10g)添加从约0.1纳克(10x10-10g)至约10纳克(10x10-9g)的可检测的标记物DNA的范围。
每千克纤维素材料(10g)添加从约1皮克(1x10-12g)至约100微克(100x10-6g)的可检测的标记物DNA的范围。
每千克纤维素材料(10g)添加从约1飞克(10-15g)至约1微克(10-6g)的可检测的标记物DNA的范围。
每千克纤维素材料(103g)添加从约10飞克(10x10-15g)至约100纳克(100x10-9)的可检测的标记物DNA的范围。
每千克纤维素材料(103g)添加从约100飞克(100x10-15g)至约10纳克(10x10-9)的可检测的标记物DNA的范围。
每千克纤维素材料(10g)添加从约1皮克(1x10-12g)至约1纳克(1x10-9g)的可检测的标记物DNA的范围。
本文所述的任何最小值可与本文所述的任何最大值组合以产生所有可能的范围。
具有唯一的核苷酸序列的可检测的标记物DNA可以包含过量的天然基因组序列的载体核酸,或随机合成或天然核酸序列的混合物。以这种方式,在无法获得用于PCR的同源PCR引物对或取决于所用的检测方法的互补核苷酸杂交探针的情况下,总核酸的提取将不会显示可检测的标记物DNA序列。
在本发明的方法中使用的可检测的标记物DNA可以是任何合适的标记物DNA。DNA可以是单链或双链DNA。在一个实施方式中,可检测的标记物DNA的单链长度可以从约20个碱基至约5,000Kb,双链长度可以从约20个碱基对至约5Kb碱基对。
碱活化
如在本文中所用的可检测的标记物DNA可在经由纤维素介质将标记物引入纤维素材料之前进行碱活化。
在一个实施方式中,在本发明的方法中使用的可检测的标记物DNA可以是碱性活化的,如Berrada等人的美国专利申请公开US 20140256881Al“Alkaline Activation ForImmobilization of DNA Taggants”中所述。其全部公开内容在此通过引证结合于本文中。
在一个实施方式中,通过将可检测的标记物DNA与具有高pH的碱性溶液混合来产生碱性条件,例如碱性溶液的pH可以是约9.0或更高的pH;约10.0或更高的pH;约11.0或更高的pH,或甚至约12.0或更高的pH,并使已经暴露于碱性条件的脱氧核糖核酸与纤维素介质接触。在一个实施方式中,碱性溶液是碱金属氢氧化物的溶液。
在一个实施方式中,该方法包括将可检测的标记物DNA暴露于碱性条件下,包括使已经暴露于碱性条件的脱氧核糖核酸与纤维素介质接触;其中碱性条件是通过将可检测的标记物DNA与碱金属氢氧化物溶液混合而产生的,碱金属氢氧化物溶液具有从约1mM至约1.0M的浓度。
可替代地,碱金属氢氧化物溶液可具有从约10mM至约0.9M的浓度。在一个实施方式中,碱金属氢氧化物溶液可具有从约0.1M至约0.8M的浓度。在另一个实施方式中,碱金属氢氧化物溶液可具有从约0.4M至约0.8M的浓度。在另一个实施方式中,碱金属氢氧化物溶液可具有约0.6M的浓度。
在一个实施方式中,将可检测的标记物DNA与具有从约为9.0至约14.0的碱性溶液混合,并在约5℃至约55℃的温度下孵育以产生碱性条件。可替代地,可检测的标记物DNA可以与具有从约为9.0至约14.0的碱性溶液混合,并在约0℃至约65℃的温度下孵育以产生碱性条件并将混合物温育约1分钟至约6小时。在另一个实施方式中,可以立即将碱处理的可检测的标记物DNA添加到纤维素介质中,例如但不限于,碱性处理的可检测的标记物DNA可以在将纤维素介质纺纱成纤维或制成纤维素薄膜之前立即添加到纤维素浴中的纤维素介质中。
在一个实施方式中,NaOH可用于碱性活化用于掺入含水核酸。作为在一些纤维素工艺中存在NaOH的潜在结果,核酸可经由副反应变为碱性活化的。因此,NaOH可用于通过中和pH来防止溶解的纤维素“凝结”。此外,可以采用其他苛性碱溶液,例如氢氧化钾、氧化钙、醇盐和/或丁基锂。
非活化的DNA
向纤维素材料中添加NMMO(N-甲基吗啉N-氧化物),将溶解纤维素材料以形成纤维素介质(纤维素涂料)。在纤维素材料的溶解工艺之后,可检测的标记物DNA在再聚合/纺纱步骤之前或期间被掺入纤维素介质中以用于标记和认证目的。在该实施方式中,可检测的标记物DNA将不会被碱性活化。
在一个示例性实施方式中,可检测的标记物DNA不是碱性活化的,并且在纤维素材料溶解之后,但在再聚合/纺纱步骤之前或期间立即添加到包含木浆、NMMO和水的纤维素介质中。在这种情况下,可检测的标记物DNA可以作为与保护剂饱和结合的复合物递送到纤维素介质中,保护剂选自以下化合物:非芳族烷基胺诸如三-丁基胺、芳族(三苯基)烷基胺诸如结晶紫或甲基绿、生物胺类诸如亚精胺或精胺。保护剂用于保护可检测的标记物DNA免于由纤维素介质(包括但不限于NMMO)的各个方面引起的降解。
已知金属离子,尤其是二价金属离子催化核酸的水解降解。因此,应尽可能避免在水和添加剂中添加这些金属离子。通常通过添加螯合剂可以除去地下水中常见的低浓度二价金属离子。
使用低浓度的约1mM至约20mM的螯合剂诸如Tris-EDTA用于隔离金属离子已被充分证实:参见例如Fischer等人的"Metal Ion/Buffer Interactions",((1979)Eur.J.Biochem.vol.94:523-530。
可替代地,水软化剂(例如氨基酸诸如谷氨酸和组氨酸,或有机二羧酸诸如苹果酸,和多肽诸如植物螯合肽等)可用于隔离和或螯合金属离子,尤其是二价金属离子。
水质可能是导致DNA可检测的标记物缺乏稳定性的原因:在许多情况下发现这可以通过用螯合剂除去二价金属离子改善水质来补救。
掺入可检测的标记物DNA
将可检测的标记物DNA表面涂覆到纤维素产品上将可检测的标记物DNA暴露于任一进一步处理和下游加工,这可以导致加工过程中存下来的可检测的标记物DNA的量减少,但这可以通过加大初始加载到纤维素产品的表面上的可检测的标记物DNA的量来解决。
通过包封在纤维素产品内而不是涂覆到纤维素产品的表面上而掺入可检测的标记物DNA保护了可检测的标记物DNA并保留了通过标准方法(诸如PCR和等温扩增进行认证)扩增DNA的能力。在另一个实施方式中,可检测的DNA标记物均匀地整合到纤维素纤维核心中,从而保护其免于进一步的下游加工。这种包封可能需要更苛刻的条件来提取可检测的DNA标记物以进行充分和可靠的检测。
可以在制备纤维素产品的任何阶段经由添加到纤维素介质中将可检测的DNA标记物添加到纤维素材料中。在一个示例性的工艺中,可检测的DNA标记物可以通过在紧接着纺纱/再聚合成纤维素纤维之前的阶段添加到纤维素介质中,或通过狭缝挤出以形成纤维素膜而添加到纤维素材料中。该方法提供在贯穿纤维素纤维或纤维素膜中掺入可检测的标记物DNA的纤维素产品。可检测的标记物DNA存在于纤维或膜的内部以及表面上,并且因此它至少部分地不受纤维素产品可能暴露的任何进一步的严苛处理。
可替代地,可将可检测的DNA标记物施加到纤维素纤维或纤维素膜的表面上。可检测的DNA标记物的较高负载量可用于在表面处理后提供可检测的DNA标记物的更大可恢复性,这可能导致一些可检测的DNA标记物的丢失。
在另一个实施方式中,本发明提供了一种认证纤维素产品的方法,包括:添加可检测的标记物诸如例如,但不限于,编码与生产过程和/或纤维素产品有关的信息的可检测的核酸,在生产纤维素产品的工艺中的步骤期间掺入到纤维素介质中;从而将该可检测的标记物掺入该纤维素产品中,以提供可检测标记的纤维素产品。将该可检测标记的纤维素产品引入至商业流中;在可检测标记的纤维素产品的纤维素介质中检测可检测的标记物的存在;并且从而认证该纤维素产品。
在另一个实施方式中,本发明提供了一种认证纤维素产品的方法,其包括:在纺纱或成膜纤维素产品之前或期间将可检测的核酸标记物添加到纤维素介质中;从而将该可检测的核酸标记物掺入该纤维素产品中,以提供可检测标记的纤维素产品;将该可检测标记的纤维素产品引入至商业流中;在可检测标记的纤维素产品的纤维素介质中检测可检测的核酸标记物的存在;并且从而认证该纤维素产品。纤维素产品可以是任何纤维素产品,诸如例如纸,或纤维素纤维,例如人造丝,或纤维素薄膜诸如玻璃纸,多孔纤维素过滤器,或弹性纤维素海绵。
可检测的核酸标记物可以是具有唯一的核苷酸序列的可检测的DNA标记物。在一个实施方式中,可检测的DNA标记物的唯一的核苷酸序列可用于编码与生产纤维素产品的过程有关的信息。在纤维素生产工艺期间添加纤维素介质之前,可检测的DNA标记物可以是或可以不是碱活化的,并且可以传递关于纤维素产品的特定信息,诸如例如但不限于生产批号、日期、时间和制造商身份。
本发明进一步提供用于认证的可检测标记的纤维素产品,包括纤维素介质和可检测的标记物,诸如掺入至纤维素介质和/或纤维素产品的表面上以形成可检测标记的纤维素产品的核酸标记物。
如果本说明书中引用的定义与通过引证并入本文的专利或出版物中提供的定义之间存在冲突,则使用本文提供的定义。
本文公开的每篇参考文献、专利和公布的专利申请的公开内容均通过引证将其整体并入本文中。
虽然已经参考本发明的示例性实施方式示出和描述了本发明,但是本领域普通技术人员将理解,在不脱离本发明的精神和范围的情况下,可以在形式和细节上进行各种改变。
实施例
实例1莱赛尔纤维涂料(纤维素材料)的DNA标记:
在室温下将木浆与50%NMMO、50%水的限定质量过量溶液混合以形成纤维素介质。然后加热该纤维素介质以使纤维素溶剂化并蒸发过量的水以形成纤维素介质。
在制造工艺期间,在两(2)个不同时间之一时将包含可检测的标记物DNA的DNA浓缩物添加到纤维素介质中:可检测的DNA标记物与纤维素材料的最终质量比通常在0.1纳克至10微克/千克纤维素材料之间。添加点是:
A.在加热期开始时添加可检测的DNA标记物。
B.在加热期后,就在挤压/纺纱之前添加可检测的DNA标记物以形成纤维。
实例2从莱赛尔纤维中回收DNA
可以使用来自莱赛尔的四种DNA回收和分析方法。
方法1
纤维的两步原位PCR,然后是标准CE(毛细管电泳):
-基于每次测试使用@10mg(即10μL)纤维。将纤维直接添加到40uL PCR反应中
在pH为8或更高下,在90℃下进行纤维的水萃取,然后进行电荷转换磁珠浓缩,然后进行PCR/CE:
-基于每次测试使用@100mg(即100μL)纤维。
方法2
在pH为8或更高下,在90℃下进行纤维的水萃取,然后进行电荷转换磁珠浓缩,然后进行qPCR:
-基于每次测试使用@100mg(即100μL)纤维。优化的DNA TaqMan测定可以在qPCR装置上展开。
方法3
将纤维在24%NaOH中在90℃下进行溶剂化10分钟,然后用乙酸盐和Nynal磁珠浓缩进行中和,然后进行qPCR:
-基于每次测试使用@100mg(即100μL)纤维。优化的DNA TaqMan测定可以在qPCR装置上展开。
方法4
将纤维在50%NMMO,50%水中在90℃下进行溶剂化,然后用乙酸盐和Nynal磁珠浓缩进行中和,然后进行qPCR:
-基于每次测试使用@100mg(即100μL)纤维。优化的DNA TaqMan测定可以在qPCR装置上展开。
Claims (18)
1.一种标记纤维素产品用于认证的方法,其包括:
在纺纱步骤之前或期间或者在加工纤维素产品的成膜步骤之前或期间,将可检测的DNA标记物添加到纤维素介质中,所述可检测的DNA标记物不是碱性活化的;以及
从而将所述可检测的DNA标记物掺入并嵌入至所述纤维素产品中以提供核酸标记的纤维素产品,
其中所述纤维素介质包含木浆、水和N-甲基吗啉氧化物。
2.根据权利要求1所述的方法,其中所述可检测的DNA标记物掺入贯穿所述纤维素产品中。
3.根据权利要求2所述的方法,其中所述可检测的DNA标记物掺入至所述纤维素产品的表面上并嵌入其中。
4.根据权利要求1所述的方法,其中所述可检测的DNA标记物以每千克纤维素材料1纳克至1微克DNA范围的量添加到所述纤维素介质中。
5.根据权利要求1所述的方法,其中所述可检测的DNA标记物以每千克纤维素材料0.1纳克至10微克DNA范围的量添加到所述纤维素介质中。
6.根据权利要求3所述的方法,其中所述可检测的DNA标记物的独特的DNA序列编码与用于生产所述纤维素产品的过程相关的信息。
7.根据权利要求6所述的方法,其中与用于生产所述纤维素产品的过程相关的信息包括生产批号、日期、时间和制造商中的一个或多个。
8.根据权利要求1所述的方法,其中所述纤维素产品是纤维素纤维。
9.根据权利要求8所述的方法,其中所述纤维素纤维是莱赛尔纤维。
10.根据权利要求1所述的方法,其中所述纤维素产品渗入至制造的产品中。
11.一种认证纤维素产品的方法,其包括:
在纺纱步骤之前或期间或者在加工纤维素产品的成膜步骤之前或期间,将可检测的DNA标记物添加到纤维素介质中,所述可检测的DNA标记物不是碱性活化的;以及
从而将所述可检测的DNA标记物掺入至所述纤维素产品中以提供核酸标记的纤维素产品;
将所述核酸标记的纤维素产品引入至商业流中;
在所述核酸标记的纤维素产品的所述纤维素介质中,检测所述DNA标记物的存在;以及
从而认证所述纤维素产品,
其中所述纤维素介质包含木浆、水和N-甲基吗啉氧化物。
12.根据权利要求11所述的方法,其中所述可检测的DNA标记物以每千克纤维素材料1纳克至1微克DNA范围的量添加到所述纤维素介质中。
13.根据权利要求11所述的方法,其中所述可检测的DNA标记物以每千克纤维素材料0.1纳克至10微克DNA范围的量添加到所述纤维素介质中。
14.根据权利要求11所述的方法,其中所述可检测的DNA标记物的独特的DNA序列编码与用于生产所述纤维素产品的过程相关的信息。
15.根据权利要求14所述的方法,其中与用于生产所述纤维素产品的过程相关的信息包括生产批号、日期、时间和制造商中的一个或多个。
16.根据权利要求11所述的方法,其中所述纤维素产品是纤维素纤维。
17.根据权利要求16所述的方法,其中所述纤维素纤维是莱赛尔纤维。
18.一种用于认证的可检测标记的纤维素产品,其包含:
纤维素介质以及在纤维素产品中和/或在纤维素产品上的可检测的DNA标记物,所述可检测的DNA标记物不是碱性活化的,
其中所述纤维素介质包含木浆、水和N-甲基吗啉氧化物。
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US10519605B2 (en) | 2019-12-31 |
EP3442719A4 (en) | 2019-11-20 |
US20200199820A1 (en) | 2020-06-25 |
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