开放性实验:聚乙烯亚胺修饰碳点的合成、纯化与表征

doi:10.3724/SP.J.1123.2023.12017

色谱 ›› 2024, Vol. 42 ›› Issue (4): 393-398.DOI: 10.3724/SP.J.1123.2023.12017

• 教学研究 • 上一篇

开放性实验:聚乙烯亚胺修饰碳点的合成、纯化与表征

李瑞¹, 许贯虹¹, 于海琳¹, 岑瑶¹, 彭艳¹, 沈凡丽², 魏芳弟¹^,^*()

1.南京医科大学, 江苏南京 211166
2.江苏省食品药品监督检验研究院, 江苏南京 210019

收稿日期:2023-12-15 出版日期:2024-04-08 发布日期:2024-04-03
通讯作者: 魏芳弟
基金资助:
南京医科大学教育研究课题(2023ZD006);南京医科大学研究生优质教育资源建设项目(2023E004)

Opening experiments: synthesis, purification, and characterization of polyethyleneimine-modified carbon dots

LI Rui¹, XU Guanhong¹, YU Hailin¹, CEN Yao¹, PENG Yan¹, SHEN Fanli², WEI Fangdi¹^,^*()

1. Nanjing Medical University, Nanjing 211166, China
2. Jiangsu Institute for Food and Drug Control, Nanjing 210019, China

Received:2023-12-15 Online:2024-04-08 Published:2024-04-03
Contact: WEI Fangdi
Supported by:
Education Research Project of Nanjing Medical University(2023ZD006);High-quality Graduate Education Resource Project of Nanjing Medical University(2023E004)

摘要/Abstract

摘要：

开放性实验是培养拔尖创新人才的有效手段。我们基于学生兴趣、科研热点和实验室条件,设计了实验方案。实验采用一步水热法,以柠檬酸(CA)为碳源,聚乙烯亚胺(PEI)为修饰剂,合成PEI修饰碳点(PEI-CDs)。首先,将CA、PEI在0.1 mol/L的盐酸中超声至完全溶解,混匀后转移到高压反应釜中,放入烘箱130 ℃反应2 h,制得PEI-CDs原液;然后将冷却至室温的原液旋转蒸发浓缩至2 mL,并用无水乙醇沉淀、洗涤;最后,将所得沉淀放入真空干燥箱,70 ℃干燥12 h得到PEI-CDs粉末。利用紫外-可见分光光度计、荧光分光光度计、红外光谱仪和透射电镜对所合成的PEI-CDs进行表征。结果表明,所采用的无水乙醇沉淀纯化方法简单、快速、经济、绿色,制得的PEI-CDs水溶性好,发光性能优异,大小均一,稳定性高。通过该开放性实验,学生不仅熟悉了大型仪器的使用,而且增强了科学研究的兴趣。

关键词: 开放性实验, 聚乙烯亚胺, 碳点, 荧光, 纯化方法

Abstract:

Open experiments are an effective means of cultivating top-notch innovative talents. Based on student interests, research hotspots and our laboratory conditions, an experimental scheme was designed. In this experiment, polyethyleneimine modified carbon dots (PEI-CDs) were prepared via a one-step hydrothermal method using citric acid (CA) as the carbon source and PEI as the surface passivator. First, CA and PEI were completely dissolved in 0.1 mol/L HCl and transferred into an autoclave. The autoclave was heated to 130 ℃ for 2 h. PEI-CDs solution was obtained. After cooling to room temperature, the solution was concentrated to 2 mL by rotary evaporation. Finally, the PEI-CDs were precipitated, washed with ethanol, and dried under vacuum at 70 ℃ for 12 h. The obtained PEI-CDs were characterized by fluorescence spectrophotometry, absorption spectrophotometry, infrared spectrometry, and transmission electron microscopy. The results indicated that anhydrous-ethanol precipitation is a simple, rapid, economical, and green purification method. The as-prepared PEI-CDs had unique properties, such as good water solubility, high luminescence, uniform particle sizes, and good stability. Through this open experiment, students can not only master the operation of large-scale instruments but also enhance their interest in scientific research.

Key words: open experiment, polyethyleneimine (PEI), carbon dots (CDs), fluorescence, purification method

中图分类号:

O658

李瑞, 许贯虹, 于海琳, 岑瑶, 彭艳, 沈凡丽, 魏芳弟. 开放性实验:聚乙烯亚胺修饰碳点的合成、纯化与表征[J]. 色谱, 2024, 42(4): 393-398.

LI Rui, XU Guanhong, YU Hailin, CEN Yao, PENG Yan, SHEN Fanli, WEI Fangdi. Opening experiments: synthesis, purification, and characterization of polyethyleneimine-modified carbon dots[J]. Chinese Journal of Chromatography, 2024, 42(4): 393-398.

图/表 8

图 1 PEI-CDs在超纯水中的(a)荧光光谱图和 (b)紫外-可见光谱图

Fig. 1 (a) Fluorescence and (b) UV-vis absorption spectra of polyethyleneimine modified carbon dots (PEI-CDs) in ultrapure water

图 2 硫酸奎宁和PEI-CDs的量子产率标准曲线

Fig. 2 Photoluminescent quantum yield (PLQY) standard curves of quinine sulfate and PEI-CDs

图 3 PEI-CDs的傅里变换叶红外光谱图

Fig. 3 FT-IR spectrum of PEI-CDs

图 4 PEI-CDs的XPS能谱图

Fig. 4 XPS spectra of PEI-CDs a. Full survey XPS spectrum; b,c,d. high-resolution XPS peaks of C 1s, N 1s, O 1s, respectively.

表 1 PEI-CDs的元素分析

Table 1 Element contents of PEI-CDs

Name	Peak/eV	Element content/%
C 1s	284	60.15
N 1s	398	18.91
O 1s	531	20.94

图 5 PEI-CDs的透射电镜图

Fig. 5 TEM images of PEI-CDs

图 6 PEI-CDs的粒径分布图

Fig. 6 Size distribution histogram of PEI-CDs

图 7 PEI-CDs在(a)紫外光照射下和(b)4 ℃下荧光强度的变化(n=3)

Fig. 7 Evolution of fluorescence intensities of PEI-CDs under (a) irradiation with ultraviolet light and (b) 4 ℃ (n=3)

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开放性实验:聚乙烯亚胺修饰碳点的合成、纯化与表征

Opening experiments: synthesis, purification, and characterization of polyethyleneimine-modified carbon dots

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