CN111821471A - 一种抗氧化MXenes材料的制备方法 - Google Patents
一种抗氧化MXenes材料的制备方法 Download PDFInfo
- Publication number
- CN111821471A CN111821471A CN202010930828.2A CN202010930828A CN111821471A CN 111821471 A CN111821471 A CN 111821471A CN 202010930828 A CN202010930828 A CN 202010930828A CN 111821471 A CN111821471 A CN 111821471A
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- Prior art keywords
- mxene
- alc
- max phase
- putting
- rapamycin
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
本发明提供了一种抗氧化MXenes材料的制备方法,其特征在于,所述纳米药物载体指负载雷帕霉素和紫杉醇的MXene二维纳米材料,其中,所述MXene载体进行聚乙二醇表面修饰,所述雷帕霉素和紫杉醇通过RGD多肽共价结合在所述纳米药物载体表面;包括以下步骤:将MAX陶瓷中M代表的部分金属粉末、M对应的碳化物或氮化物和过量铝粉混合进行球磨、压制,在通入氩气的条件下,进行高温烧结,得到MAX相陶瓷材料;再加入TEOS,于80℃下反应,离心、洗涤,得介孔氧化硅包裹的MXene纳米片;再用RGD多肽共价结合,负载药物,即得。本发明可以实现对肿瘤的靶向治疗,并获得良好抑瘤效果。
Description
技术领域
本发明涉及纳米材料领域和生物技术领域,具体涉及一种负载雷帕霉素和紫杉醇药物的二维纳米材料MXene的制备方法。
背景技术
近年来,MXenes作为一种新型的二维层状材料,因其独特的层状结构、亲水性、电子电导、化学稳定性好,以及不同电解质离子插层等特点,自2011年发展至今收到了广大科研工作者的极大关注,特别是Ti3AlC2作为MXenes家族中被研究最深的一员,在电化学电容器和锂离子电池上均展现了极广泛的应用前景。Mxenes是由德雷赛尔大学的Yury Gogosti和Michel W.Barsoum在2011年研制出来的一种新型二维层状结构的过渡金属碳化物或氮化物材料,具有许多与石墨烯相似的性质,目前已发现的MXene材料约70种,包括Ti3C2、Ti2C、V2C、Nb2C、Nb4C3、Ta4C3和Ti4N3等,MXenes在材料领域有着极大的潜力,制备MXenes材料最为典型的方法是,利用HF溶液选择性地剥离MAX相中的A层,从而获得二维MXenes纳米材料。MAX相结构由Mn+1Xn层和A原子层依次交错排列而成[1]-[3]。由于M-X是以共价/金属/离子混合的强键结合,而M-A是以较弱的金属键结合,因此可以利用M-A与M-X在键结合方式以及相对强度上的差异,使A原子被选择性腐蚀而不破坏M-X键[4]。
目前DES常用的涂层药物有两种:雷帕霉素与紫杉醇。雷帕霉素是一种大环内酯类免疫抑制剂,可与免疫蛋白FKBP12(FK506-binding protein 120)结合形成FKBP12雷帕霉素复合体,然后结合到特定的细胞周期调节蛋白mTOR,抑制mTOR的活性,二mTOR在细胞周期G1走向S期中发挥重要作用,最终抑制细胞分裂、增值。紫杉醇也具有抑制细胞增值的作用,其通过结合微管蛋白二聚体的β亚族结合,从而抑制了有细胞分裂激素激活的、负责微管解聚作用的蛋白激酶,进而产生了牢固的微管,抑制了纺锤丝的形成和有丝分裂。
浙江工业大学在申请公布号为CN107537540A的中国专利中提供了一种MXene(Ti3C2)负载钯催化剂及其制备方法和应用。
山东大学在申请公布号为CN102579402B的中国专利中提供了一种负载紫杉醇囊泡的制备方法。
深圳市移丽环保股份有限公司在申请公布号为CN105943521B的中国专利提供了一种硅藻土负载紫杉醇的功能无纺布芯片。
山东大学齐鲁医院在申请公布号为CN104707170A的中国专利中提供了一种钛材表面制备纳米级羟基磷灰石负载雷帕霉素药物的方法。
三峡大学在申请号为CN105997938A的中国专利中提供了一种载紫杉醇和/或载siRNA微泡的制备方法和应用。
深圳先进技术研究院在申请号为CN104758240A的中国专利中国提供了一种转载紫杉醇的纳米药物复合体及其制备方法。
华侨大学在申请号为CN105386155A的中国专利中提供了一种担载紫杉醇的串珠状纳米纤维及其制备方法。
桂林电子科技大学在申请号为CN102961345A的中国专利中提供了一种雷帕霉素/磁性羧甲基壳聚糖纳米载药微球的制备方法。
阿布拉克斯生物科学有限公司在申请号为US104814930B美国专利中发表《作为抗癌剂的包含雷帕霉素和白蛋白的纳米颗粒》,该发明以通过给予包括雷帕霉素或其衍生物的纳米颗粒来治疗、稳定、预防和/或延迟癌症的方法为特征,提供包含含有载体蛋白和雷帕霉素或其衍生物的纳米颗粒的组合物(例如单位剂型)。还提供了治疗癌症的联合治疗方法,包括给予个体有效量的含雷帕霉素或其衍生物的纳米颗粒和第二疗法。
发明内容
针对现有技术的不足,本发明提供了一种抗氧化MXenes材料的制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种抗氧化MXenes材料的制备方法,包括以下步骤:
①将钛粉、过量的铝粉和石墨粉混合进行球磨、压制,在通入氩气的条件下,进行高温烧结,得到Ti3AlC2陶瓷材料;②将步骤①所得物碎成粉末,置于氢氟酸中反应,离心洗涤后,置于氢氧化四丙基铵水溶液中反应,离心、洗涤,得到Ti3C2MXenes材料;③将Ti3C2MXenes材料水溶液滴入CTAC和TEA的混合水溶液中反应;再加入TEOS,于80℃下反应,离心、洗涤,得介孔氧化硅包裹的MXene纳米片;④对步骤③物进行聚乙二醇表面修饰,再用RGD多肽共价结合,负载药物,即得。
具体步骤为:
步骤一 使用球磨装置研磨M所代表的金属粉末、M对应的碳化物或氮化物粉末和Al粉末,以1:2:1(质量比)的比例在70 rpm下研磨18 h;
步骤二 随后把球研磨的前驱体粉末装进一个氧化铝坩埚,覆盖上石墨箔,然后放入管式炉,在室温下用氩气净化炉30分钟;
步骤三 将前驱体粉末加热到1380℃,在约100 sccm的氩气流量下保持2小时。升温和降温速率均为3℃/min;
步骤四 Al-Ti3AlC2的烧结块随后使用镀锡钻头进行研磨,以生成MAX粉,随后使用9M的HCl进行清洗,直到不产生气泡。一般情况下,500ml 9 M HCl足以清洗50 - 60g Al-Ti3AlC2;
步骤五 通过真空过滤装置过滤Al-Ti3AlC2/HCl混合物,加去离子水清洗。(过滤膜孔径5微米,过滤的清液呈深紫色);
步骤六 过滤后的MAX在80℃的真空烤箱中干燥至少6小时;
步骤七 干燥后的Al-Ti3AlC2再通过450目(32支座m)颗粒筛进行筛分。为刻蚀成MXene做准备;
步骤八 称取步骤七所制得的原料:按照摩尔分数比,MAX相陶瓷:氯离子盐或溴离子盐:NaCL:KCl=1:1-6:3:3;将称好的原料在球墨设备中充分球墨混合均匀;
步骤九 熔盐反应刻蚀MAX相陶瓷:将步骤八中按比例称取球磨好的反应原料,放入氧化铝反应坩埚中在真空或者惰性气体的气氛在550-850℃的保温2到5小时后冷却 ;
步骤十 洗涤净化反应产物:将步骤九的反应产物放入10%的稀盐酸中浸泡1小时超声清洗震荡静置1小时后取下层沉淀物重复3次,将盐酸清洗后的反应产物用去离子水反复的离心清洗直到PH为6,最后离心后取沉淀物倒掉上清液,将去离子水清洗得到的产物在真空干燥箱中以45℃的温度烘干20小时后即为多层Mxene材料;
步骤十一 对步骤十所得的MXene材料进行聚乙二醇表面修饰,再用RGD多肽共价结合,加入雷帕霉素或紫杉醇负载,即可得到负载雷帕霉素或紫杉醇的MXene纳米材料;
本发明制得的负载药物的MXene材料具有分散性好,均匀性强,生物相容性好等优点
本发明可以实现对肿瘤的靶向治疗,并获得良好抑瘤效果。
附图说明
图1为Al过量Nb2AlC MAX相陶瓷;
图2为高温刻蚀后的多层Nb2C MXene;
图3为TBAOH插层剥离后的少层Nb2C MXene;
图4为抗氧化Mxene 和非抗氧化Mxene的效果对比图;
具体实施案例
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
请参阅图1-4,本发明提供一种技术方案:在本实施例中,通过以下方法制备Nb2CMXene载体,并负载雷帕霉素:分别取5gNb、10gNb2C和5gAl粉放入求磨装置中充分研磨研磨;随后将混合粉末放入坩埚,放进管式炉中通入氩气后加热到1380℃,20小时后取出,得到MAX相前驱体;将该烧结的结块研磨成粉末,用9M的盐酸清洗,直至不在产生气泡;随后使用真空抽滤装置进行抽滤,加去离子水清洗;过滤后的粉末置于真空烤箱中干燥6小时;取10gMAX相前驱体,6gCuCl2,7.8gNaCl和9.9gKCl充分研磨混合均匀;将混合粉末放入管式炉中通入氩气在700℃保持5小时;取出后将反应产物放入10%的稀盐酸中浸泡1小时超声清洗震荡静置1小时后取下层沉淀物重复3次,将盐酸清洗后的反应产物用去离子水反复的离心清洗直到PH为6,最后离心后取沉淀物倒掉上清液,将去离子水清洗得到的产物在真空干燥箱中以45℃的温度烘干20小时后即得到Nb2C MXene材料;将所得的Nb2C MXene材料进行聚乙二醇表面修饰,再用RGD多肽共价结合,加入雷帕霉素负载,得到负载雷帕霉素的Nb2CMXene材料。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (9)
1.一种抗氧化MXenes材料的制备方法,其特征在于,所述纳米药物载体指负载雷帕霉素和紫杉醇的MXene二维纳米材料,其中,所述MXene载体进行聚乙二醇表面修饰,所述雷帕霉素和紫杉醇通过RGD多肽共价结合在所述纳米药物载体表面;
根据权利要求1所述的MXene载体的制备方法,其特征在于,包括以下步骤:
过量添加Al法制备MAX相前驱体,MAX相是一类三元层状金属陶瓷材料的统称,这类化合物具有统一的化学式Mn+1AXn,其中M是早起过渡金属,A是III、IV主族元素,X是C或者N,n代表1,2,3等;将M所代表的金属粉末、M对应的碳化物或氮化物粉末和Al粉末(其中加入的Al粉过量)混合放入球磨装置球磨,将研磨好的粉末装入氧化铝坩埚中,放入管式炉中在惰性气氛下高温煅烧,将煅烧后的结块研磨以生成MAX相,随后用盐酸清洗;过滤清洗后干燥,即可得到Al-Ti3AlC2 MAX相前驱体;
熔盐法刻蚀MAX相材料合成MXene 材料
称取MAX相原料、氯离子盐或溴离子盐、NaCl和KCl,将其放入球磨设备中充分球磨混合均匀,随后将研磨好的粉末放入氧化铝坩埚中,放入管式炉中在惰性气氛下高温反应后冷却,将反应产物放入稀盐酸中浸泡,之后超声清洗震荡静置,取沉淀物,用去离子水反复离心清洗即可得到多层MXene材料;
MXene材料负载药物
由步骤(2)得到的MXene材料,将其水溶液滴入CTAC和TEA的混合水溶液中反应;再加入TEOS,于80℃下反应,离心、洗涤,得介孔氧化硅包裹的MXene纳米片,对得到的纳米片进行聚乙二醇表面修饰,再用RGD多肽共价结合,负载药物,即可得到负载药物的MXene纳米材料, 所述的负载药物为雷帕霉素和紫杉醇中的至少一种。
2.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(1)中,过渡金属包括但不限于Sc、Ti、V、Cr、Zr、Nb、Hf、Ta,对应的质量比为1:2:1,其中一种反应物粉末搭配为Ti、TiC和Al粉末的质量比为1:2:1,所制得的Max相陶包含并不仅限于Ti2AlC、Ti2AlN、V2AlC、V2AlN、Nb2AlC、NbAl2N、Ta2AlC、Ti3AlC2、Ti3AlN2、V3AlC2、Ta3AlC2、Ta3AlN2、 Ti4AlC3、Ti4AlN3、Ta4AlC3、Ta4NAl3、Nb4AlC3 中的任意一种或两种以上的MAX相陶瓷组合;所述步骤(1)中,球磨在70 rpm下研磨18 h,惰性气氛为氩气,氧化铝坩埚盖上石墨箔,管式炉先用氩气净炉30min,加热温度为1380℃,氩气流量约为100sccm,持续2小时,加热和降温速率为3℃/min。
3.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(1)中,HCl浓度为9M,清洗到不再产生气泡。
4.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(1)中,干燥的环境为80℃,时间至少6小时。
5.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(2)中,所述的氯离子盐或溴离子盐包括AgCl 、CuBr2、、ZnBr2 、CoBr2、FeBr2 、NiBr2 、NaCl、KCl中的任意一种或两种以上的组合。
6.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(2)中,所述的MAX相原料与氯离子盐或溴离子盐、NaCl和KCl的摩尔分数比为1:1~6:3:3,所述的惰性气氛为氩气,反应的温度控制在550-850℃,反应时间为2-5小时。
7.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(2)中,所述的盐酸为10%的稀盐酸,浸泡时间为1小时。
8.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(2)中,超声清洗后静置时间为1小时,然后取下层沉淀物,此步骤重复3次。
9.根据权利要求2所述的MXene载体制备方法,其特征在于,所述步骤(2)中,用去离子水反复离心清洗,直到pH为6,最后倒掉上清液,取出沉淀物,将所得沉淀物放入真空干燥箱中以45℃烘干20小时,即可得到多层MXene材料。
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