淡竹叶碳量子点的微波法制备及在细胞成像中的应用探究 增强出版

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"name": [ { "lang": "zh", "surname": "徐", "givenname": "长妍", "namestyle": "eastern", "prefix": "" }, { "lang": "en", "surname": "XU", "givenname": "Chang-yan", "namestyle": "eastern", "prefix": "" } ], "stringName": [], "aff": [ { "rid": "aff1", "text": "1" }, { "rid": "aff2", "text": "2" }, { "rid": "aff3", "text": "3" } ], "role": [ "corresp" ], "corresp": [ { "rid": "cor1", "lang": "en", "text": "E-mail： changyanxu1999@163.com", "data": [ { "name": "text", "data": "E-mail： changyanxu1999@163.com" } ] } ], "bio": [ { "lang": "zh", "text": [ "徐长妍（1967-），女，江苏南京人，博士，教授，2000年于南京林业大学获得博士学位，主要从事生物质基碳量子点绿色制备、石墨烯绿色制备、高阻隔性绿色包装材料等的研究。 E-mail: changyanxu1999@163.com" ], "graphic": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818370&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818378&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818374&type=", "width": "24.89200020", 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Science and Engineering， Nanjing Forestry University， Nanjing 210000， China" } ] } ] }, { "id": "aff2", "intro": [ { "lang": "zh", "label": "2", "text": "南京林业大学 江苏省林产品高效加工利用联合创新中心， 江苏 南京　210000", "data": [ { "name": "text", "data": "南京林业大学 江苏省林产品高效加工利用联合创新中心， 江苏 南京　210000" } ] }, { "lang": "en", "label": "2", "text": "Jiangsu Co-innovation Centre of Efficient Processing and Utilization of Forest Products， Nanjing Forestry University， Nanjing 210000， China", "data": [ { "name": "text", "data": "Jiangsu Co-innovation Centre of Efficient Processing and Utilization of Forest Products， Nanjing Forestry University， Nanjing 210000， China" } ] } ] }, { "id": "aff3", "intro": [ { "lang": "zh", "label": "3", "text": "南京林业大学 绿色生物质燃料与化学品江苏省重点实验室， 江苏 南京　210000", "data": [ { "name": "text", "data": "南京林业大学 绿色生物质燃料与化学品江苏省重点实验室， 江苏 南京　210000" } ] }, { "lang": "en", "label": "3", "text": "Jiangsu Province Key Laboratory of Green Biomass-based Fuels and Chemicals， Nanjing Forestry University， Nanjing 210000， China", "data": [ { "name": "text", "data": "Jiangsu Province Key Laboratory of Green Biomass-based Fuels and Chemicals， Nanjing Forestry University， Nanjing 210000， China" } ] } ] }, { "id": "aff4", "intro": [ { "lang": "zh", "label": "4", "text": "2019年江苏省研究生工作站：靖江国林木业有限公司 （工作站编号：2019_099）， 江苏 靖江　214500", "data": [ { "name": "text", "data": "2019年江苏省研究生工作站：靖江国林木业有限公司 （工作站编号：2019_099）， 江苏 靖江　214500" } ] }, { "lang": "en", "label": "4", "text": "2019 Jiangsu Graduate Workstation： Jingjiang Guolin Wood Industry Co.， Ltd.（Workstation No. 2019_099）， Jingjiang 214500， China", "data": [ { "name": "text", "data": "2019 Jiangsu Graduate Workstation： Jingjiang Guolin Wood Industry Co.， Ltd.（Workstation No. 2019_099）， Jingjiang 214500， China" } ] } ] } ] }, "abstracts": [ { "lang": "zh", "data": [ { "name": "p", "data": [ { "name": "text", "data": "利用响应曲面法 （RSM）系统研究了微波作用时间 （" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "）、微波功率 （" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "）、淡竹叶与去离子水的料液比 （" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "）对微波法制备淡竹叶氮硅自掺杂碳量子点 （N/Si⁃CQDs）荧光量子产率 （QY）的影响。得到了上述工艺参数对QY的影响显著性次序以及对应的QY回归模型与最佳工艺参数，通过验证实验证明优化结果可靠。采用最佳工艺得到的N/Si⁃CQDs的平均粒径较小且分布均匀，在水中分散性良好，具有激发依赖的发射特性，荧光稳定性较高，对HEK293细胞具有较低细胞毒性，且可被细胞吸收而照亮细胞从而明确区分细胞质和细胞核，说明该碳量子点可用于细胞成像。该研究不仅为淡竹叶的高值化利用提供了一个新思路，而且对提高生物质碳量子点的微波法制备效率、促进其在细胞成像等生物医学领域的应用具有参考价值。" } ] } ] }, { "lang": "en", "data": [ { "name": "p", "data": [ { "name": "text", "data": "In this study， response surface methodology（RSM） was used to study the effects of microwave action time （" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "）， microwave power（" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "） and the ratio of common lophatherum herb to deionized water （" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "）" }, { "name": "italic", "data": [ { "name": "text", "data": " " } ] }, { "name": "text", "data": "on the fluorescence quantum yield （QY） of N/Si-CQDs prepared by microwave method. The significance order of the influence of the above process parameters on QY， and the corresponding QY regression model and the best process parameters are obtained， and the optimization results are proved to be reliable through validation experiments. The average particle size of N/Si-CQDs obtained by the best process is small and evenly distributed， with good dispersion in water， excitation dependent emission characteristics， high fluorescence stability， low cytotoxicity to HEK293 cells. And the N/Si CQDs can be absorbed by cells to illuminate cells， so as to clearly distinguish cytoplasm and nucleus， which shows that the N/Si-CQDs can be used for cell imaging. This study not only provides a new idea for the high-value utilization of bamboo leaves， but also has reference value for improving the efficiency of microwave preparation of biomass carbon quantum dots and promoting their application in biomedical fields such as cell imaging." } ] } ] } ], "keyword": [ { "lang": "zh", "data": [ [ { "name": "text", "data": "淡竹叶" } ], [ { "name": "text", "data": "碳量子点" } ], [ { "name": "text", "data": "微波法" } ], [ { "name": "text", "data": "响应曲面法" } ], [ { "name": "text", "data": "细胞成像" } ] ] }, { "lang": "en", "data": [ [ { "name": "text", "data": "common lophatherum herb" } ], [ { "name": "text", "data": "carbon quantum dots" } ], [ { "name": "text", "data": "microwave method" } ], [ { "name": "text", "data": "response surface method" } ], [ { "name": "text", "data": "cell imaging" } ] ] } ], "highlights": [], "body": [ { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "1　引　　言" } ], "level": "1", "id": "s1" } }, { "name": "p", "data": [ { "name": "text", "data": "碳量子点 （Carbon quantum dots，CQDs）是一种零维碳基纳米材料，具有良好的生物相容性和优异的光致发光性能" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "1", "type": "bibr", "rid": "R1", "data": [ { "name": "text", "data": "1" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，被广泛应用于细胞成像" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "2", "type": "bibr", "rid": "R2", "data": [ { "name": "text", "data": "2" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、药物传递" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "3", "type": "bibr", "rid": "R3", "data": [ { "name": "text", "data": "3" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、离子检测" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "4", "type": "bibr", "rid": "R4", "data": [ { "name": "text", "data": "4" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "等领域。碳量子点的物理化学性质受碳源和制备方法的直接影响，如杂原子的引入，可以改善CQDs的性质" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "5", "type": "bibr", "rid": "R5", "data": [ { "name": "text", "data": "5" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。生物质材料一般具有丰富的杂原子，可实现CQDs合成过程中的杂原子自掺杂，无需引入新的掺杂剂或者经过繁杂的钝化过程即可实现杂原子诱导而形成新的表面态，从而提高CQDs的荧光量子产率和荧光强度" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "6", "type": "bibr", "rid": "R6", "data": [ { "name": "text", "data": "6" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "7", "type": "bibr", "rid": "R7", "data": [ { "name": "text", "data": "7" } ] } } ], "rid": [ "R6", "R7" ], "text": "6-7", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。此外，生物质碳源还具有环保、成本低、来源广泛的优点，还可以一定程度上替代昂贵的化学试剂" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "8", "type": "bibr", "rid": "R8", "data": [ { "name": "text", "data": "8" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "9", "type": "bibr", "rid": "R9", "data": [ { "name": "text", "data": "9" } ] } } ], "rid": [ "R8", "R9" ], "text": "8-9", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。近年来，一些生物质碳源如葡萄籽" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "5", "type": "bibr", "rid": "R5", "data": [ { "name": "text", "data": "5" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、西兰花" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "6", "type": "bibr", "rid": "R6", "data": [ { "name": "text", "data": "6" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和大蒜" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "10", "type": "bibr", "rid": "R10", "data": [ { "name": "text", "data": "10" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "等已被用于合成杂原子掺杂的CQDs，且凭借其生物相容性良好、细胞毒性较低、荧光稳定性良好而在细胞成像等领域体现出良好的应用潜力。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "碳量子点的合成方法包括微波法" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "11", "type": "bibr", "rid": "R11", "data": [ { "name": "text", "data": "11" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、水热法" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "12", "type": "bibr", "rid": "R12", "data": [ { "name": "text", "data": "12" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、激光销蚀法" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "13", "type": "bibr", "rid": "R13", "data": [ { "name": "text", "data": "13" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和电弧放电法" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "14", "type": "bibr", "rid": "R14", "data": [ { "name": "text", "data": "14" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "等。其中，微波法相对于其他CQDs制备方法，是一种应用广泛、绿色、快速、高效的碳量子点制备方法，通过高频率电磁波作用，在短时间内使碳量子点的碳源发生碳化、裂解从而达到快速制备碳量子点的目的" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "15", "type": "bibr", "rid": "R15", "data": [ { "name": "text", "data": "15" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。但是，通过微波法制备的CQDs目前仍然存在粒径分布不均匀、性能可控性较差等问题" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "16", "type": "bibr", "rid": "R16", "data": [ { "name": "text", "data": "16" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，这主要是因为其制备工艺参数的选取不合理所致。现有有关微波法制备CQDs工艺参数优化的研究多采用正交试验设计方法，虽然可以在一定程度上优化CQDs制备工艺，但不能用于系统分析各个因素对响应值的影响主次顺序、各因素两两组合的交互作用、对指定工艺下制备的碳点进行性能预判" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "11", "type": "bibr", "rid": "R11", "data": [ { "name": "text", "data": "11" } ] } }, { "name": "text", "data": "," }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "15", "type": "bibr", "rid": "R15", "data": [ { "name": "text", "data": "15" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "16", "type": "bibr", "rid": "R16", "data": [ { "name": "text", "data": "16" } ] } } ], "rid": [ "R15", "R16" ], "text": "15-16", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。因此，科学优化CQDs的微波法制备工艺对于提高微波法制备CQDs的效率、改善CQDs的结构和性能从而促进其应用具有重要意义。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "淡竹叶 （Lophatherum gracile）是一种药食同源的多年生草本植物，广泛分布于中国、日本、韩国等亚洲国家" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "17", "type": "bibr", "rid": "R17", "data": [ { "name": "text", "data": "17" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "19", "type": "bibr", "rid": "R19", "data": [ { "name": "text", "data": "19" } ] } } ], "rid": [ "R17", "R18", "R19" ], "text": "17-19", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，已被中国食品添加剂标准化委员会批准为功能性食品工业中的天然添加剂" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "20", "type": "bibr", "rid": "R20", "data": [ { "name": "text", "data": "20" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。淡竹叶富含的类黄酮、多糖、酚酸等生物活性物质和矿质元素赋予其良好的药理作用，为建立具有良好生物相容性的CQDs的活性功能基团提供了机会" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "21", "type": "bibr", "rid": "R21", "data": [ { "name": "text", "data": "21" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。但现阶段淡竹叶除部分茎叶得到入药利用以外，均被丢弃浪费" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "22", "type": "bibr", "rid": "R22", "data": [ { "name": "text", "data": "22" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。如何提高淡竹叶的功能化、高附加值的转换利用是该产业面临的一个难题。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "响应曲面法 （Response surface methodology，RSM）是一种所需要的试验组数相对较少的统计学试验方法，可以找出各因素水平的最佳组合，揭示试验指标与各因子间的定量规律。此外，采用该方法还可以在多元线性回归的基础上主动收集数据，获得具有较好拟合效果的回归方程的同时建立复杂多维空间曲面，使得预测较接近实际情况" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "23", "type": "bibr", "rid": "R23", "data": [ { "name": "text", "data": "23" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "经预实验发现淡竹叶的C、O、Si、N元素含量较高，是合成氮硅自掺杂碳量子点 （N/Si-CQDs）的理想材料，而利用淡竹叶制备CQDs的相关研究还未见公开报道" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "24", "type": "bibr", "rid": "R24", "data": [ { "name": "text", "data": "24" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。值得注意的是，生物相容性和地球丰富度俱佳的氮 （N）和硅 （Si）元素，近年来由于适宜的原子大小、化学价态以及化学惰性和低毒性的优点，在CQDs掺杂过程中，易于引入多种官能团，提供更多的活性位点，产生更多的表面缺陷，可以获得较高的量子产率和荧光强度，因而在CQDs掺杂领域受到广泛关注" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "4", "type": "bibr", "rid": "R4", "data": [ { "name": "text", "data": "4" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "7", "type": "bibr", "rid": "R7", "data": [ { "name": "text", "data": "7" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "12", "type": "bibr", "rid": "R12", "data": [ { "name": "text", "data": "12" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。但现阶段随着杂原子的加入，引起了CQDs的粒径增大，且由于掺杂CQDs的粒径大小在细胞毒性与荧光特性方面起着重要的影响作用，CQDs的粒径控制与尺寸均匀性不佳，在一定程度上限制了CQDs的实际使用。 而近年来发展的极小CQDs （指粒径小于3 nm的CQDs）由于平均粒径较小、粒径分布均匀，在生物医学等诸多领域展现出更好的效果" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "9", "type": "bibr", "rid": "R9", "data": [ { "name": "text", "data": "9" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。因此，本研究将淡竹叶作为唯一原料，以响应曲面法优化极小N/Si-CQDs的微波法制备工艺，并采用步骤简单、应用广泛的CCK-8实验来评估N/Si-CQDs对转染效率高、增长速度快、对外界微环境较为敏感的HEK293细胞的细胞毒性" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "25", "type": "bibr", "rid": "R25", "data": [ { "name": "text", "data": "25" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，探索其在细胞成像中的应用潜力。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2　实　　验" } ], "level": "1", "id": "s2" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.1　实验材料" } ], "level": "2", "id": "s2a" } }, { "name": "p", "data": [ { "name": "text", "data": "实验材料见表S1，所有试剂均为分析纯，无需进一步纯化即可使用。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2　N/Si‐CQDs的微波法制备" } ], "level": "2", "id": "s2b" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2.1 实验方案" } ], "level": "3", "id": "s2b1" } }, { "name": "p", "data": [ { "name": "text", "data": "采用微波法制备淡竹叶氮硅自掺杂碳量子点 （N/Si-CQDs）的工艺参数优化包括两步。首先，以N/Si-CQDs的荧光量子产率 （QY）为评价指标，结合已有研究" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "1", "type": "bibr", "rid": "R1", "data": [ { "name": 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"name": "text", "data": "按照表S2中微波作用时间 （" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "）、微波功率 （" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "）和淡竹叶与去离子水的料液比 （" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "）的取值，采用以下步骤制备N/Si-CQDs：第一步，使用250 mL的烧杯盛装，选择指定料液比的淡竹叶粉末与分散剂 （去离子水10 mL）；第二步，利用磁力搅拌器 （MYP11-2，上海梅颖浦仪器仪表制造有限公司，中国）搅拌10 min，转速为500 r/min，使淡竹叶粉充分分散在水中，并将烧杯放入微波炉 （G90F23CN3LV-C2 （S5）, Galanz, China）中进行微波处理；第三步，取出烧杯，加入30 mL去离子水搅拌，得到反应液，使用0.22 µm滤微孔滤膜纯化，以去除残留物和大颗粒，并将过滤的反应液利用离心机 （H-1650, Cence, China）以10 000 r/min转速离心15 min，得到的上清液即为N/Si-CQDs水溶液；第四步，将上述N/Si-CQDs水溶液冷冻1 d后 （-20 ℃），采用真空冷冻干燥机 （Alpha 1-2 LDplus, BMH, China）在-60 ℃下干燥处理3 d，得到固体N/Si-CQDs，用于配制指定浓度的N/Si-CQDs水溶液及后续表征。所有试验均重复3次。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.3　N/Si‐CQDs的性能表征" } ], "level": "2", "id": "s2c" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.3.1　N/Si-CQDs的物理形貌表征" } ], "level": "3", "id": "s2c1" } }, { "name": "p", "data": [ { "name": "text", "data": "采用高倍率透射电子显微镜 （JEM-2100 UHR, JEOL, Japan）表征N/Si-CQDs的物理形貌。采用滴管将配制的N/Si-CQDs分散液 （0.5 mg/mL）滴于超薄碳支撑膜上，自然晾干后，使用高倍率透射电子显微镜观察N/Si-CQDs的形貌。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.3.2　N/Si-CQDs的化学结构表征" } ], "level": "3", "id": "s2c2" } }, { "name": "p", "data": [ { "name": "text", "data": "采用拉曼光谱仪 （HORIBA LabRAM., HR Evolution, Fr）、傅里叶变换红外光谱仪 （Nicolet iS10, Thermo Electron Corp., Madison, WI, USA）和 X 射线光电子能谱仪 （AXIS Ultra ADLD, Shimadzu, Japan）表征N/Si-CQDs的化学结构。取N/Si-CQDs粉末 （2 mg）与纯KBr（200 mg）研细均匀，压片 （厚度1 mm，直径13 nm），即可用于测定红外光谱。取N/Si-CQDs粉末（0.1 g），压片（厚度1 mm，直径5 nm），即可用于测定XPS，结合能根据 284.6 eV 的C 1s峰校准。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.3.3　N/Si-CQDs的光致发光特性表征" } ], "level": "3", "id": "s2c3" } }, { "name": "p", "data": [ { "name": "text", "data": "分别通过荧光分光光度计 （LS55, Perkin-Elmer, USA）和紫外分光光度计 （LAMBDA950, Perkin-Elmer, USA）在扫描速度均为300 nm/min的条件下，获得配制的N/Si-CQDs水溶液 （0.5 mg/mL）的荧光光谱和紫外-可见吸收光谱。本研究将获得的荧光光谱峰值数据最大时所对应的激发波长定义为N/Si-CQDs的最佳激发波长。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "根据" }, { "name": "xref", "data": { "text": "公式 （1）", "type": "disp-formula", "rid": "DF1", "data": [ { "name": "text", "data": "公式 （1）" } ] } }, { "name": "text", "data": "计算N/Si-CQDs的荧光量子产率QY （" }, { "name": "italic", "data": [ { "name": "text", "data": "η" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "QY" } ] }, { "name": "text", "data": "）" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "26", "type": "bibr", "rid": "R26", "data": [ { "name": "text", "data": "26" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。选择溶解在 0.1 mol/L 硫酸中的硫酸奎宁作为参比物 （" }, { "name": "italic", "data": [ { "name": "text", "data": "η" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "QY" } ] }, { "name": "text", "data": " = 54%），在激发波长360 nm处分别测定参比物和N/Si-CQDs水溶液样品的荧光光谱和吸光度曲线。" } ] }, { "name": "dispformula", "data": { "label": [ { "name": "text", "data": "（1）" } ], "data": [ { "name": "math", "data": { "math": "", "graphicsData": { "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818402&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818397&type=", "width": "39.45466614", "height": "8.63599968", "fontsize": "" } } }, { "name": "text", "data": " ，" } ], "id": "DF1" } }, { "name": "p", "data": [ { "name": "text", "data": "其中，" }, { "name": "italic", "data": [ { "name": "text", "data": "η" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "QY" } ] }, { "name": "text", "data": "为N/Si-CQDs的荧光量子产率；" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "text", "data": "为测得的荧光光谱的积分面积，下标R代表参比物，X代表 N/Si-CQDs样品；" }, { "name": "italic", "data": [ { "name": "text", "data": "A" } ] }, { "name": "text", "data": "为360 nm激发波长处的吸光度；" }, { "name": "italic", "data": [ { "name": "text", "data": "η" } ] }, { "name": "text", "data": "为折射率，在本研究中，" }, { "name": "italic", "data": [ { "name": "text", "data": "η" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "X" } ] }, { "name": "text", "data": "/" }, { "name": "italic", "data": [ { "name": "text", "data": "η" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "=1。荧光量子产率是研究弛豫过程和光化学历程的重要参数，它表示物质将吸收的光能转化成荧光的性能。荧光量子产率也与物质的化学结构有关，在定量的光化学中，荧光量子产率是一个十分有用的参量" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "26", "type": "bibr", "rid": "R26", "data": [ { "name": "text", "data": "26" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "碳量子点的荧光稳定性直接关系到在生物成像领域的应用效果，因此，本研究还探讨了N/Si-CQDs的荧光稳定性，主要考察了紫外光（365 nm）照射与氯化钠浓度以及不同pH对N/Si-CQDs荧光强度的影响，即N/Si-CQDs的抗光漂白性试验、抗盐性试验和N/Si-CQDs在不同pH条件下的稳定性实验" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "27", "type": "bibr", "rid": "R27", "data": [ { "name": "text", "data": "27" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "28", "type": "bibr", "rid": "R28", "data": [ { "name": "text", "data": "28" } ] } } ], "rid": [ "R27", "R28" ], "text": "27-28", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。在N/Si-CQDs的抗光漂白性试验中，先将配制的N/Si-CQDs水溶液 （0.5 mg/mL）密封于透明离心管并放置在暗室中，使用紫外灯持续照射不同时间 （0，1，2，3，4，5，6 h）后，再利用荧光分光光度计记录N/Si-CQDs溶液在最佳激发波长处的荧光光谱数据；在N/Si-CQDs的抗盐性实验中，为考察N/Si-CQDs受共存分子和离子的干扰情况，在pH=7的条件下分别在配制的N/Si-CQDs水溶液 （0.5 mg/mL）中加入不同克重的NaCl，使NaCl的浓度达到指定值 （0，0.02，0.04，0.06，0.08，0.1 mol/mL），再记录N/Si-CQDs在不同NaCl浓度下在最佳激发波长处的荧光光谱数据；在N/Si-CQDs在不同pH条件下的稳定性实验中，为考察N/Si-CQDs的荧光强度受不同pH条件的干扰情况，本研究将荧光光谱数据中的峰值定义为N/Si-CQDs的荧光强度 （FL）。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.4　N/Si-CQDs的细胞毒性试验与细胞成像试验" } ], "level": "2", "id": "s2d" } }, { "name": "p", "data": [ { "name": "text", "data": "培养基配制：先将胎牛血清在56 ℃下灭活0.5 h，然后配制10%胎牛血清血清和1%双抗的培养基；胰蛋白酶配制：精确称定0.25 g胰蛋白酶到100 mL容量瓶中，加磷酸盐缓冲液 （PBS）溶解定容；细胞悬液配制：细胞株中加入上述配制培养基，置于培养箱中培养 （37 ℃，5% CO" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "），每隔24 h换液，待细胞密度达到70%~90%。用胰蛋白酶将细胞消化为细胞悬液。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "细胞毒性试验：采用CCK-8试剂盒测定N/Si-CQDs对人胚胎肾细胞 （HEK293）的毒性。先将预先制备好的HEK293细胞悬液按每孔100 μL加入到96孔培养板，每孔细胞密度为1×10" }, { "name": "sup", "data": [ { "name": "text", "data": "5" } ] }, { "name": "text", "data": "个；然后将培养板在细胞培养箱预培养 （37 ℃，5% CO" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "）24 h，再从培养箱里取出。每孔加入10 μL不同质量浓度（12.5，20，50，100，200 μg/mL）的N/Si-CQDs溶液（以无菌去离子水配制）后，放回培养箱 （37 ℃，5% CO" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "）持续孵育24 h。从培养箱里取出培养板，再向每孔加入10 μL的CCK-8溶液，再次放回培养箱（37 ℃，5% CO" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "）孵育2 h。拿出培养板，用酶标仪测定在450 nm处的吸光度。按照" }, { "name": "xref", "data": { "text": "公式（2）", "type": "disp-formula", "rid": "DF2", "data": [ { "name": "text", "data": "公式（2）" } ] } }, { "name": "text", "data": "计算细胞存活率（Cell viability）" }, { "name": "italic", "data": [ { "name": "text", "data": "V" } ] }, { "name": "bold", "data": [ { "name": "sup", "data": [ { "name": "text", "data": " " } ] }, { "name": "sub", "data": [ { "name": "text", "data": "C" } ] } ] }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "29", "type": "bibr", "rid": "R29", "data": [ { "name": "text", "data": "29" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "：" } ] }, { "name": "dispformula", "data": { "label": [ { "name": "text", "data": "（2）" } ], "data": [ { "name": "math", "data": { "math": "", "graphicsData": { "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818408&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818404&type=", "width": "50.46133423", "height": "4.57200003", "fontsize": "" } } }, { "name": "text", "data": "，" } ], "id": "DF2" } }, { "name": "p", "data": [ { "name": "text", "data": "其中，" }, { "name": "italic", "data": [ { "name": "text", "data": "A" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "s" } ] }, { "name": "text", "data": "为实验孔吸光度（含有细胞、培养基、CCK-8溶液、N/Si-CQDs溶液），" }, { "name": "italic", "data": [ { "name": "text", "data": "A" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "c" } ] }, { "name": "text", "data": "为对照孔吸光度 （含有细胞、培养基、CCK-8溶液、不含N/Si-CQDs溶液），" }, { "name": "italic", "data": [ { "name": "text", "data": "A" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "b" } ] }, { "name": "text", "data": "为空白孔吸光度 （含培养基、CCK-8溶液、不含细胞、N/Si-CQDs溶液）。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "细胞成像实验：先将预先制备好的细胞悬液接种到含有培养基的6孔培养板中，再将培养板在培养箱预培养24 h（37 ℃，5% CO" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "），然后用磷酸盐缓冲溶液 （PBS）缓冲液 （pH=7.4）洗涤细胞。将浓度为200 µg/mL的N/Si-CQDs溶液加入孔中，并进一步孵育24 h。然后，用磷酸盐缓冲溶液 （PBS）（pH=7.4）洗涤三次，去除多余的没有进入细胞的N/Si-CQDs，并使用共聚焦激光扫描显微镜 （NIKON Eclipse Ti,NIKON, Japan）系统在405 nm激发波长下观察细胞形态及荧光成像情况。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3　结果与讨论" } ], "level": "1", "id": "s3" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.1　N/Si-CQDs的微波法制备工艺优化" } ], "level": "2", "id": "s3a" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.1.1　单因素试验" } ], "level": "3", "id": "s3a1" } }, { "name": "p", "data": [ { "name": "text", "data": "如" }, { "name": "xref", "data": { "text": "图1", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1" } ] } }, { "name": "text", "data": "（a）~（c）所示，本研究通过控制单一变量分别得到了三因素 （" }, { "name": "italic", "data": [ { "name": "text", "data": "T、W、R" } ] }, { "name": "text", "data": "）对荧光量子产率 （QY）的影响。随着微波时间自5 min增加至25 min，QY数值呈现出明显的先增大后减小的变化趋势，且在" }, { "name": "italic", "data": [ { "name": "text", "data": "T=" } ] }, { "name": "text", "data": "15 min时QY达到最高值1.34%（" }, { "name": "xref", "data": { "text": "图1", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1" } ] } }, { "name": "text", "data": "（a））。当" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "由200 W增加至600 W时，QY由1.10%增至1.37%；但当" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "继续从600 W增至　1 000 W时，QY反而由1.37%缓慢降低至1.36%（" }, { "name": "xref", "data": { "text": "图1", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1" } ] } }, { "name": "text", "data": "（b））。此外，随着" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "由5 mg/mL增至25 mg/mL，QY也呈现先增大后减小的变化趋势，且在　" }, { "name": "italic", "data": [ { "name": "text", "data": "R=" } ] }, { "name": "text", "data": "20 mg/mL时QY达到最高值1.54%（" }, { "name": "xref", "data": { "text": "图1", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1" } ] } }, { "name": "text", "data": "（c））。综上所述，在微波法合成N/Si-CQDs的过程中，需要经过“氧化分解-交联-碳化”过程。为了使氧化分解发生，需要一定的温度和反应时间阈值，这与微波功率及微波作用时间密切相关" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "15", "type": "bibr", "rid": "R15", "data": [ { "name": "text", "data": "15" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。在单因素实验中，我们发现，相对较低的功率和较短的反应时间可以触发前驱体碳材料初步形成N/Si-CQDs碳核结构，具有相对较低的荧光；而功率的提升和反应时间的延长，往往使得前驱体进一步碳化，这造成了碳量子点材料表面官能团破坏与粒子聚集等，从而降低其荧光。综合考虑三因素" }, { "name": "italic", "data": [ { "name": "text", "data": "T、W、R" } ] }, { "name": "text", "data": "对评价指标QY的影响，后续响应曲面优化设计选择" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "的范围为 10~20 min，步长为5；" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "的范围为400~800 W，步长为200；" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "的范围为15~25 mg/mL，步长为5。" } ] }, { "name": "fig", "data": { "id": "F1", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图1" } ], "title": [ { "name": "text", "data": "单因素试验结果分析： （a）" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "， （b）" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "， （c）" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.1" } ], "title": [ { "name": "text", "data": "Analysis of single factor test results：（a）" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "， （b）" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "， （c）" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818410&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818417&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818413&type=", "width": "60.04931641", "height": "147.26634216", "fontsize": "" } ] } } ] }, { "name": 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"name": "text", "data": "P" } ] }, { "name": "text", "data": "<" }, { "name": "text", "data": "0.001）显著，失拟项（" }, { "name": "italic", "data": [ { "name": "text", "data": "P" } ] }, { "name": "text", "data": "=0.112 2" }, { "name": "text", "data": ">" }, { "name": "text", "data": "0.05）" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "30", "type": "bibr", "rid": "R30", "data": [ { "name": "text", "data": "30" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "表明失拟项相对于绝对误差不显著。因此，该模型对试验的拟合程度良好，能较好地反映各因素与响应值之间的真实关系，可以利用该模型对实验参数进行分析。由" }, { "name": "italic", "data": [ { "name": "text", "data": "F" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "P" } ] }, { "name": "text", "data": "值的大小可以推断，在所选择的试验范围内，3个因素对QY影响的顺序为：" }, { "name": "italic", "data": [ { "name": "text", "data": "T>R>W" } ] }, { "name": "text", "data": "。二次项" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "sup", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "、" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "sup", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "和" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "sup", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "的影响极显著，一次项" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "、" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "也达到极显著水平，表明各提取工艺参数对量子产率的影响不是简单线性关系" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "31", "type": "bibr", "rid": "R31", "data": [ { "name": "text", "data": "31" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。根据回归方程得到模拟的响应曲面图及相应的等高线图，如" }, { "name": "xref", "data": { "text": "图2", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2" } ] } }, { "name": "text", "data": "（a）~（f）所示，响应面的坡度越大，等高线的形状越接近椭圆形，说明响应面对该影响因素有较高的敏感度" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "32", "type": "bibr", "rid": "R32", "data": [ { "name": "text", "data": "32" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，即对QY影响较大。" } ] }, { "name": "fig", "data": { "id": "F2", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图2" } ], "title": [ { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": " （ （a）～ （b））、" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": " （ （c）～ （d））、" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": " （ （e）～（f））对QY的影响。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.2" } ], "title": [ { "name": "text", "data": "（a）， （b）Influence of " }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": " and " }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": " on QY. （c）， （d）Influence of " }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": " and " }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": " on QY. （e）， （f）Influence of " }, { "name": "italic", "data": [ { "name": "text", "data": "W " } ] }, { "name": "text", "data": "and " }, { "name": "italic", "data": [ { "name": "text", "data": "R " } ] }, { "name": "text", "data": "on QY." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818427&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818432&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818430&type=", "width": "78.51599121", "height": "101.13110352", "fontsize": "" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "如" }, { "name": "xref", "data": { "text": "图2", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2" } ] } }, { "name": "text", "data": "（a）～（f）所示，QY随着三因素（" }, { "name": "italic", "data": [ { "name": "text", "data": "T、W、R" } ] }, { "name": "text", "data": "）的变化趋势均呈现出一定弧度，但随" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "因素变化，响应曲面变化更大，" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "因素次之，随" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "因素响应曲面变化最小，说明" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "比" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "对量子产率具有更显著的影响" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "23", "type": "bibr", "rid": "R23", "data": [ { "name": "text", "data": "23" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "32", "type": "bibr", "rid": "R32", "data": [ { "name": "text", "data": "32" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，与方差分析结果一致。响应面分析得到最优工艺为：" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "为14.056 min、" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "为618.52 W、" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "为19.8 mg/mL（10 mL去离子水），此时QY达到1.632%。考虑到试验的可行性与设备实际调节范围，我们选择" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "为14 min、" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "为600 W、" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "为19.8 mg/mL（10 mL去离子水），进行 3 次平行验证试验，其平均QY值为1.625%，与理论QY值 （1.632%）相对偏差仅为0.215%，表明试验数据与模型预测响应值的拟合性良好，证明该模型真实可信。因此，在后续的碳量子点结构和性能表征中，只选择在上述最优工艺条件下制得的N/Si-CQDs为研究对象。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.2　N/Si‐CQDs的结构与性能" } ], "level": "2", "id": "s3c" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.2.1　N/Si‐CQDs的物理形貌和化学结构" } ], "level": "3", "id": "s3c1" } }, { "name": "p", "data": [ { "name": "text", "data": "本研究采用高分辨率透射电子显微镜 （TEM）研究了N/Si-CQDs的尺寸和形貌。如" }, { "name": "xref", "data": { "text": "图3", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3" } ] } }, { "name": "text", "data": "所示，N/Si-CQDs均匀分布在水中，其颗粒多为球形，具有典型的非晶态碳质结构，无明显晶格" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "33", "type": "bibr", "rid": "R33", "data": [ { "name": "text", "data": "33" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。使用Nano measurer软件随机选取100个颗粒测量粒径，得到N/Si-CQDs的平均粒径为1.35 nm。与现有报道中采用微波法制备的生物质碳量子点相比，本研究制备的N/Si-CQDs粒径更小、粒径分布更窄，这更有利于其在细胞成像等领域的应用" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "34", "type": "bibr", "rid": "R34", "data": [ { "name": "text", "data": "34" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。为进一步了解N/Si-CQDs分子结构研究，采用拉曼光谱法分析，如图S1所示，在1 342 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和1 588 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "处存在两个主要峰值，分别是D-峰和G-峰" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "27", "type": "bibr", "rid": "R27", "data": [ { "name": "text", "data": "27" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。D-峰和G-峰的强度比（" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "text", "data": "（D）/" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "text", "data": "（G））约为1.31，表明合成的N/Si-CQDs结构中存在大量的无定形碳，与上述TEM结果相互印证。" } ] }, { "name": "fig", "data": { "id": "F3", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图3" } ], "title": [ { "name": "text", "data": "N/Si-CQDs的透射电镜图，插图： N/Si-CQDs的粒径分布图。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.3" } ], "title": [ { "name": "text", "data": "TEM image. Inset： particle size distribution of N/Si-CQDs" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818437&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818443&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818442&type=", "width": "76.70068359", "height": "76.48117065", "fontsize": "" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "本研究借助红外光谱和XPS光谱两种表征手段，分析了前驱体淡竹叶与N/Si-CQDs所含元素、官能团和化学键，如图S2、图S3、" }, { "name": "xref", "data": { "text": "图4", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4" } ] } }, { "name": "text", "data": "和" }, { "name": "xref", "data": { "text": "图5", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5" } ] } }, { "name": "text", "data": "所示。在" }, { "name": "xref", "data": { "text": "图4", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4" } ] } }, { "name": "text", "data": "中，3 270.39 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "处的宽峰对应于N—H键的拉伸振动或O—H伸缩振动，较宽峰的原因是：N、O的较强电负性导致其所对应的—NH" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "与—OH官能团可与溶H" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "O形成氢键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "35", "type": "bibr", "rid": "R35", "data": [ { "name": "text", "data": "35" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。在2 933.55 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "附近的峰表明N/Si-CQDs结构中存在C—H伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "36", "type": "bibr", "rid": "R36", "data": [ { "name": "text", "data": "36" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "；2 130.86 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "附近区域的峰表明N/Si-CQDs结构中存在炔烃的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "37", "type": "bibr", "rid": "R37", "data": [ { "name": "text", "data": "37" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "；在1 574.09 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的峰对应C=C键或N—H键的拉伸振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "35", "type": "bibr", "rid": "R35", "data": [ { "name": "text", "data": "35" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "；在1 361.12 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": " 处的吸收峰归因于C—H键的弯曲振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "38", "type": "bibr", "rid": "R38", "data": [ { "name": "text", "data": "38" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "；在1 107.70 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": " 和1 041.83 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": " 处的峰则应属于Si—O和Si—N键伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "7", "type": "bibr", "rid": "R7", "data": [ { "name": "text", "data": "7" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。与前驱体淡竹叶的的红外光谱、XPS图谱对比可知，经水相微波反应后，N/Si-CQDs相较于前驱体，亲水性官能团含量提升，Si—O、Si—N等化学键大量生成，由此形成了N/Si-CQDs复杂表面态。" } ] }, { "name": "fig", "data": { "id": "F4", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图4" } ], "title": [ { "name": "text", "data": "N/Si-CQDs的FT-IR光谱" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.4" } ], "title": [ { "name": "text", "data": "FT-IR spectrum of N/Si-CQDs" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818447&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818453&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818451&type=", "width": "62.36560059", "height": "51.87185669", "fontsize": "" } ] } }, { "name": "fig", "data": { "id": "F5", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图5" } ], "title": [ { "name": "text", "data": "（a）N/Si-CQDs的XPS谱；（b）N/Si-CQDs的元素含量； （c）C 1s的高分辨率XPS谱；（d）N 1s的高分辨率XPS谱；（e） O 1s的高分辨率XPS谱；（f）Si 2p的高分辨率XPS谱。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.5" } ], "title": [ { "name": "text", "data": "XPS of the N/Si-CQDs（a）， element content（b）， C 1s（c）， N 1s（d）， O 1s（e） and Si 2p（f） spectra of the N/Si-CQDs." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818458&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818464&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818460&type=", "width": "128.58398438", "height": "149.10693359", "fontsize": "" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "在" }, { "name": "xref", "data": { "text": "图5", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5" } ] } }, { "name": "text", "data": "中，N/Si-CQDs的XPS全光谱显示出4个主要的特征峰，分别对应于C 1s（284.8 eV）、 N 1s（400.0 eV）、O 1s（532.2 eV）和Si 2p（102.2 eV）的结合能，这表明N/Si-CQDs含有C（72.1%）、N（1.1%）、O（23.7%）和Si（3.1%） 4种元素。通过分峰拟合操作，得到C 1s、N 1s、O 1s和Si 2p 的高分辨率 XPS 光谱（" }, { "name": "xref", "data": { "text": "图5", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5" } ] } }, { "name": "text", "data": "（c）~ （f））。其中，C 1s谱显示出284.9，286.4，288.3 eV的3个峰，分别归属于C—C" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "39", "type": "bibr", "rid": "R39", "data": [ { "name": "text", "data": "39" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、C—O" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "40", "type": "bibr", "rid": "R40", "data": [ { "name": "text", "data": "40" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和C=O键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "41", "type": "bibr", "rid": "R41", "data": [ { "name": "text", "data": "41" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。N 1s图中399.4 eV和400.2 eV处的峰分别归因于N—Si" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "42", "type": "bibr", "rid": "R42", "data": [ { "name": "text", "data": "42" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和N—H键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "41", "type": "bibr", "rid": "R41", "data": [ { "name": "text", "data": "41" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。在O 1s图中，532.3 eV处有1个拟合峰归属于C—O键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "39", "type": "bibr", "rid": "R39", "data": [ { "name": "text", "data": "39" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "；101.9 eV和102.7 eV的峰分别归属于Si—N" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "42", "type": "bibr", "rid": "R42", "data": [ { "name": "text", "data": "42" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和Si—O键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "43", "type": "bibr", "rid": "R43", "data": [ { "name": "text", "data": "43" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。总之，N/Si-CQDs的XPS谱图分析表明，其结构中含有C—C、C—O、C=O、N—H、Si—N和Si—O键等，证实了N/Si-CQDs表面存在亲水基团以及N/Si杂原子的成功掺杂，该结果与N/Si-CQDs的红外光谱分析结果相互印证。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.2.2　N/Si‐CQDs的荧光性能及荧光稳定性" } ], "level": "3", "id": "s3c2" } }, { "name": "p", "data": [ { "name": "text", "data": "N/Si-CQDs的荧光发射呈现出激发波长依赖性，如" }, { "name": "xref", "data": { "text": "图6", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6" } ] } }, { "name": "text", "data": "（a）。在370~430 nm激发波长条件下，N/Si-CQDs的荧光强度表现出先增高后降低的趋势，且当最佳激发波长为400 nm时，在400 nm的激发波长下，如" }, { "name": "xref", "data": { "text": "图6", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6" } ] } }, { "name": "text", "data": " （b）所示，N/Si-CQDs在492 nm处出现最大荧光发射峰，该发射波长位于绿光波段区域" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "44", "type": "bibr", "rid": "R44", "data": [ { "name": "text", "data": "44" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。如上所述，最佳工艺制备的N/Si-CQDs表面富含多种官能团，这些官能团可以形成缺陷位点的捕获中心" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "12", "type": "bibr", "rid": "R12", "data": [ { "name": "text", "data": "12" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。一般来说，碳量子点的荧光机制与碳量子点表面态中电子和空穴之间的辐射复合有关" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "11", "type": "bibr", "rid": "R11", "data": [ { "name": "text", "data": "11" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。即在一定激发波长条件下，本研究制备的N/Si-CQDs表面发生了电子与空穴的辐射复合，并被光捕获。因此，制备的N/Si-CQDs的荧光行为受N/Si-CQDs表面状态的支配。由目前对CQDs材料激发依赖性荧光机理探讨的报道可知，表面多种官能团的存在会在其能隙之间形成多重能级及相应的多重电子跃迁，引起CQDs材料的激发依赖行为" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "12", "type": "bibr", "rid": "R12", "data": [ { "name": "text", "data": "12" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "15", "type": "bibr", "rid": "R15", "data": [ { "name": "text", "data": "15" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。因此，本研究认为制备的N/Si-CQDs复杂的表面态导致了激发态的多样性，即不同表面官能团的存在导致不同跃迁模式或引起多种不同能级，进而导致N/Si-CQDs的激发依赖现象。" } ] }, { "name": "fig", "data": { "id": "F6", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图6" } ], "title": [ { "name": "text", "data": "（a）不同激发波长下N/Si-CQDs的发射光谱；（b）N/Si-CQDs的紫外-可见吸收光谱和荧光光谱，插图： N/Si-CQDs水溶液分别在可见光 （左）和紫外光365 nm （右）下的照片。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.6" } ], "title": [ { "name": "text", "data": "（a）Emission spectra of N/Si-CQDs at different excitation wavelengths. （b）UV-Vis absorption spectra and fluorescence spectra of N/Si-CQDs. Inset： photograph of N/Si-CQDs aqueous solution under visible light （left） and ultraviolet light（365 nm， right）." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818468&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818472&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818469&type=", "width": "64.77978516", "height": "99.61533356", "fontsize": "" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "为了进一步阐明N/Si-CQDs的光学性质，如" }, { "name": "xref", "data": { "text": "图6", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6" } ] } }, { "name": "text", "data": "（b）所示，本研究对配制的N/Si-CQDs水溶液 （0.5 mg/mL）进行了紫外-可见吸收光谱与荧光光谱分析，N/Si-CQDs样品在260~350 nm的紫外波长范围内表现出吸收，这通常归属于C=C键的π-π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "跃迁，表明了N/Si-CQDs中共轭结构的形成" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "45", "type": "bibr", "rid": "R45", "data": [ { "name": "text", "data": "45" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。此外，由" }, { "name": "xref", "data": { "text": "图6", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6" } ] } }, { "name": "text", "data": "（b）中的插图可见，N/Si-CQDs水溶液在可见光下呈浅黄色，在365 nm紫外光下表现蓝色荧光。N/Si-CQDs具有的良好光致发光特性可能是由于芳香族sp" }, { "name": "sup", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "结构域的带隙跃迁、N/Si-CQDs的量子尺寸效应和表面缺陷所致" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "46", "type": "bibr", "rid": "R46", "data": [ { "name": "text", "data": "46" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] }, { "name": "p", "data": [ { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "为N/Si-CQDs的荧光强度（FL）" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "FL" } ] }, { "name": "text", "data": "稳定性试验结果。" }, { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "（a）的横坐标表示波长为365 nm的紫外光照射时长 （0，1，2，3，4，5，6 h），本研究将“紫外灯照射时长0 h”的荧光强度定义为" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "1FL0" } ] }, { "name": "text", "data": "。" }, { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "（a）的纵坐标表示紫外灯照射不同时长下N/Si-CQDs对应的荧光强度" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "1FL" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "1FL0" } ] }, { "name": "text", "data": "的比值，即为N/Si-CQDs经紫外灯照射不同时长后的荧光强度保留率（" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "1FL" } ] }, { "name": "text", "data": "/" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "1FL0" } ] }, { "name": "text", "data": "）。" } ] }, { "name": "fig", "data": { "id": "F7", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图7" } ], "title": [ { "name": "text", "data": "（a）365 nm紫外灯照射时间对N/Si-CQDs荧光强度的影响；（b）不同浓度的NaCl对N/Si-CQDs荧光强度的影响；（c）不同pH对N/Si-CQDs荧光强度的影响。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.7" } ], "title": [ { "name": "text", "data": "（a）Effect of illumination time under 365 nm UV light on the fluorescence intensity. （b）Effect of NaCl concentrations on the fluorescence intensity. （c）Effect of pH on the fluorescence intensity." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818476&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818481&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818477&type=", "width": "60.01544189", "height": "146.41748047", "fontsize": "" } ] } }, { "name": "p", "data": [ { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "（b）的横坐标表示NaCl水溶液浓度（0，0.02，0.04，0.06，0.08，0.1 mol/mL），本研究将“NaCl水溶液浓度为0 mol/mL”的荧光强度定义为" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "2FL0" } ] }, { "name": "text", "data": "。" }, { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "（a）的纵坐标表示N/Si-CQDs在不同浓度的NaCl水溶液中对应的荧光强度" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "2FL" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "2FL0" } ] }, { "name": "text", "data": "的比值，即为N/Si-CQDs在不同浓度的NaCl水溶液中的荧光强度保留率 （" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "2FL" } ] }, { "name": "text", "data": "/" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "2FL0" } ] }, { "name": "text", "data": "）。本研究发现制备的N/Si-CQDs在6 h紫外灯照射后，荧光强度保留率为92.25%。此外，即使氯化钠浓度高达0.1 mol/L，N/Si-CQDs的荧光强度保留率仍可达到98.90%。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "本研究将“pH=4”的荧光强度定义为" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "3FL0" } ] }, { "name": "text", "data": "，" }, { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "（c）的纵坐标表示N/Si-CQDs在不同pH水溶液中对应的荧光强度" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "3FL" } ] }, { "name": "text", "data": "与" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "3FL0" } ] }, { "name": "text", "data": "的比值，即为N/Si-CQDs在不同pH的水溶液中的荧光强度保留率 （" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "3FL" } ] }, { "name": "text", "data": "/" }, { "name": "italic", "data": [ { "name": "text", "data": "I" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "3FL0" } ] }, { "name": "text", "data": "）。如" }, { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "（c）所示，随着pH从4增加到10，N/Si-CQDs的荧光强度保留率为94.24%，FL在酸性和中性环境下几乎保持不变。由于大多数的生物活性反应发生在这个pH范围内，所以N/Si-CQDs在pH=4～10范围内的高稳定性使其在生物应用中潜力巨大" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "27", "type": "bibr", "rid": "R27", "data": [ { "name": "text", "data": "27" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "由于N/Si-CQDs溶液的荧光强度FL与N/Si-CQDs在水介质形成的胶体和其形态稳定性高度相关。因此，本研究也进行了N/Si-CQDs 7 d内的吸光度稳定性实验。我们发现，N/Si-CQDs水溶液在避光低温（4 ℃）条件下储存7 d后，吸光度基本维持不变（吸光度保持率大于98.7%），见图S4。结合上述对N/Si-CQDs物理形貌和化学结构的表征分析，本研究推测N/Si-CQDs具有较高荧光稳定性的原因是N、Si杂原子的成功掺杂诱导形成了大量的表面官能团与表面缺陷。这其中N/Si-CQDs表面亲水官能团的存在使N/Si-CQDs具有良好的水溶性；同时，N/Si-CQDs表面具有相同或近似的表面官能团与表面缺陷，容易造成N/Si-CQDs纳米粒子具有相同的表面电荷进而造成N/Si-CQDs纳米粒子间互斥，即在水中呈现出均匀单分散状态，在水介质中形成胶体并具有一定的形态稳定性。不仅提高了N/Si-CQDs的荧光量子产率与荧光强度，同时也提高了N/Si-CQDs的荧光强度稳定性" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "5", "type": "bibr", "rid": "R5", "data": [ { "name": "text", "data": "5" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "6", "type": "bibr", "rid": "R6", "data": [ { "name": "text", "data": "6" } ] } } ], "rid": [ "R5", "R6" ], "text": "5-6", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.3　N/Si⁃CQDs的细胞毒性与细胞成像分析" } ], "level": "2", "id": "s3d" } }, { "name": "p", "data": [ { "name": "xref", "data": { "text": "图8", "type": "fig", "rid": "F8", "data": [ { "name": "text", "data": "图8" } ] } }, { "name": "text", "data": "为 HEK293细胞与不同浓度N/Si-CQDs孵育24 h后的相对细胞活性。即使在较高的N/Si-CQDs浓度 （200 μg/mL）下，HEK293细胞的存活率 （92.95%）仍然超过90%，这说明淡竹叶衍生的N/Si-CQDs具有优越的生物相容性" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "36", "type": "bibr", "rid": "R36", "data": [ { "name": "text", "data": "36" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] }, { "name": "fig", "data": { "id": "F8", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图8" } ], "title": [ { "name": "text", "data": "HEK293细胞与不同浓度N/Si-CQDs孵育24 h后的相对细胞活性" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.8" } ], "title": [ { "name": "text", "data": "Cell viability of HEK293 cells in the presence of diffferent concentrations of N/Si-CQDs for 24 h" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818485&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818490&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818486&type=", "width": "62.46800232", "height": "51.15670776", "fontsize": "" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "综上所述，N/Si-CQDs展现出的良好的水分散性、高荧光稳定性以及低细胞毒性，均证明其在细胞成像领域的应用潜力" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "3", "type": "bibr", "rid": "R3", "data": [ { "name": "text", "data": "3" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "38", "type": "bibr", "rid": "R38", "data": [ { "name": "text", "data": "38" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。为此，本研究进行了体外细胞成像实验，进一步测试了N/Si-CQDs作为细胞成像剂的可行性。" }, { "name": "xref", "data": { "text": "图9", "type": "fig", "rid": "F9", "data": [ { "name": "text", "data": "图9" } ] } }, { "name": "text", "data": "为N/Si-CQDs的荧光共聚焦细胞成像图片。在含有N/Si-CQDs （200 μg/mL）的培养基中孵育24 h后，在405 nm激发下，HEK293细胞质表现出绿色荧光，细胞形态正常。由此推测，N/Si-CQDs很容易通过内吞作用被细胞吸收,具有良好的细胞通透性，并明确区分细胞质和细胞核" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "43", "type": "bibr", "rid": "R43", "data": [ { "name": "text", "data": "43" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。体外活细胞成像是研究活细胞的细胞结构和功能的重要手段，可进一步加深对细胞结构和功能的复杂性质的理解。本研究制备得到的N/Si-CQDs由于其亮度、光稳定性、可调谐的荧光发射、低毒性、廉价的制备等特性，是传统的荧光探针在细胞成像领域内的有力替代品" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "1", "type": "bibr", "rid": "R1", "data": [ { "name": "text", "data": "1" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "15", "type": "bibr", "rid": "R15", "data": [ { "name": "text", "data": "15" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。丰富的亲水表面官能团与极小的粒径使这种纳米颗粒很容易与细胞膜相互作用，并通过内吞过程进入到细胞质中" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "27", "type": "bibr", "rid": "R27", "data": [ { "name": "text", "data": "27" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，在细胞质中表现出绿色荧光，表明N/Si-CQDs可能具有标记特定的细胞器的能力，其光谱行为的变化与细胞和细胞器内的化学变化相对应的标记有望为生物医学等相关领域研究提供助力" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "1", "type": "bibr", "rid": "R1", "data": [ { "name": "text", "data": "1" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "4", "type": "bibr", "rid": "R4", "data": [ { "name": "text", "data": "4" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。N/Si-CQDs的低毒性使它们能够在细胞中无害地实现细胞成像，这一结果与前人报道的生物质CQDs具有低细胞毒性、并可运用在细胞成像领域的研究结果一致" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "2", "type": "bibr", "rid": "R2", "data": [ { "name": "text", "data": "2" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。因此，本研究制备得到的N/Si-CQDs有望作为荧光探针用于活细胞成像和其他生物医学应用。" } ] }, { "name": "fig", "data": { "id": "F9", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图9" } ], "title": [ { "name": "text", "data": "HEK293细胞与N/Si-CQDs（200 μg/mL）孵育24 h，在激发波长405 nm条件下的荧光图像。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.9" } ], "title": [ { "name": "text", "data": "Fluorescence image of HEK293 cells incubated with N/Si-CQDs（200 μg/mL） for 24 h under excitation wavelength of 405 nm" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818493&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818500&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=39818496&type=", "width": "64.29385376", "height": "54.84101868", "fontsize": "" } ] } } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "4　结　　论" } ], "level": "1", "id": "s4" } }, { "name": "p", "data": [ { "name": "text", "data": "本研究以荧光量子产率为指标，采用响应曲面法优化淡竹叶自掺杂碳量子点N/Si-CQDs的微波制备工艺，确定了微波作用时间 （" }, { "name": "italic", "data": [ { "name": "text", "data": "T" } ] }, { "name": "text", "data": "）、微波功率 （" }, { "name": "italic", "data": [ { "name": "text", "data": "W" } ] }, { "name": "text", "data": "）、淡竹叶与去离子水的料液比 （" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "）对荧光量子产率这一指标的显著性影响及其交互作用，确定了最佳工艺参数，并进行了验证实验。在实际最佳工艺条件下得到的N/Si-CQDs的水分散性良好、粒径较小且分布均匀；具有激发依赖的荧光发射；N、Si杂原子成功自掺杂使N/Si-CQDs表现出良好的荧光稳定性，在长时间的紫外照射后与NaCl浓度范围较广的水溶液中荧光强度保留率较高；由于没有化学试剂参与合成，该N/Si-CQDs即使在高浓度下也对HEK293细胞表现出较低的细胞毒性。此外，N/Si-CQDs能被HEK293细胞有效吸收，这表明该碳量子点在细胞成像等生物医学领域具有良好的应用潜力。综上所述，以淡竹叶为碳源，通过引入响应曲面法优化淡竹叶N/Si-CQDs的微波制备工艺，探究N/Si-CQDs在细胞成像中的应用价值，不仅为紧迫的废弃生物质资源的高值化转化利用提供了一条新思路，而且对于提高生物质碳量子点的微波法制备效率、促进其在细胞成像等生物医学领域的应用具有参考价值。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "本文补充文件和专家审稿意见及作者回复内容的下载地址：" }, { "name": "extlink", "data": { "text": [ { "name": "text", "data": "http://cjl.lightpublishing.cn/thesisDetails#10.37188/CJL.20220256." } ], "href": "http://cjl.lightpublishing.cn/thesisDetails#10.37188/CJL.20220256." } } ] } ] } ], "footnote": [], "reflist": { "title": [ { "name": "text", "data": "参考文献" } ], "data": [ { "id": "R1", "label": "1", "citation": [ { "lang": "en", "text": [ { "name": "text", "data": "ARCHITHA N" }, { "name": "text", "data": "， " }, { "name": "text", 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