模板法控制合成AgInSe2:Zn2+近红外荧光量子点及其生物标记应用※

doi:10.6023/A21120606

化学学报 ›› 2022, Vol. 80 ›› Issue (5): 625-632.DOI: 10.6023/A21120606 上一篇下一篇

所属专题：中国科学院青年创新促进会合辑

研究论文

模板法控制合成AgInSe₂:Zn²⁺近红外荧光量子点及其生物标记应用^※

廉纬^a^,^b, 方泽铠^a^,^b, 涂大涛^a^,^b^,^c^,^*(), 李嘉尧^a^,^b, 韩思远^b, 李仁富^b^,^c, 商晓颖^b^,^c, 陈学元^a^,^b^,^c^,^*()

a 福州大学化学学院福州 350108
b 中国科学院福建物质结构研究所中国科学院功能纳米结构设计与组装重点实验室福州 350002
c 中国科学院福建物质结构研究所结构化学国家重点实验室福州 350002

投稿日期:2021-12-30 发布日期:2022-05-31
通讯作者: 涂大涛, 陈学元
作者简介:
^※庆祝中国科学院青年创新促进会十年华诞.
基金资助:
国家自然科学基金(U1805252); 国家自然科学基金(21975257); 国家自然科学基金(22135008); 福建省自然科学基金(2019I0029); 福建省自然科学基金(2021L3024)

Template-Based Controlled Synthesis and Bioapplication of AgInSe₂:Zn²⁺ Near-Infrared Luminescent Quantum Dots^※

Wei Lian^a^,^b, Zekai Fang^a^,^b, Datao Tu^a^,^b^,^c(), Jiayao Li^a^,^b, Siyuan Han^b, Renfu Li^b^,^c, Xiaoying Shang^b^,^c, Xueyuan Chen^a^,^b^,^c()

a College of Chemistry, Fuzhou University, Fuzhou 350108, China
b CAS Key Laboratory of Design and Assembly of Functional Nanostructures, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, China
c State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, China

Received:2021-12-30 Published:2022-05-31
Contact: Datao Tu, Xueyuan Chen
About author:
^※Dedicated to the 10th anniversary of the Youth Innovation Promotion Association, CAS.
Supported by:
National Natural Science Foundation of China(U1805252); National Natural Science Foundation of China(21975257); National Natural Science Foundation of China(22135008); Natural Science Foundation of Fujian Province(2019I0029); Natural Science Foundation of Fujian Province(2021L3024)

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摘要/Abstract

AgInSe₂(AISe)量子点具有带隙小、斯托克斯位移大、荧光寿命长且不含重金属有毒元素等特性, 使其在生物医学领域具有重要研究价值. 同时, AISe量子点的光学性质对尺寸和组成具有强烈的依赖关系, 然而传统的直接合成法很难实现对AISe量子点形貌和组分的精准调控, 从而极大限制了其发光效率. 对此, 作者提出了温和条件(75 ℃)下以In₂Se₃:Zn²⁺量子点为模板, 离子交换法控制合成AISe近红外荧光量子点的策略, 所合成的AISe量子点很好地维持了In₂Se₃:Zn²⁺模板的形貌, 进一步通过系统调节Ag/In投料物质的量比控制离子交换程度, AISe量子点的实际Ag/In组分比实现了从0.26~1.09宽范围调节; 最高绝对量子产率可达42.5%, 这一数值远高于通过直接合成法所得到的AISe量子点. 通过稳态、瞬态和低温光谱等手段对不同组分AISe量子点的发光行为进行了系统的光谱学研究, 揭示了其发光机理. 另外, 利用AISe量子点高效的近红外发光和良好的生物安全性, 实现了基于AISe近红外量子点探针的肿瘤细胞靶向成像, 展示出AISe量子点在生物成像和疾病的早期诊疗等领域具有很好的应用潜力.

关键词: AgInSe₂, 近红外, 量子点, 阳离子交换, 荧光纳米探针

AgInSe₂ (AISe) quantum dots (QDs) exhibit large Stokes shift, composition-dependent photoluminescence (PL), long PL lifetimes and low toxicity, making them exceptional candidates in a wide variety of bioapplications. However, it remains notoriously challenging to precisely control both the morphology and composition to optimize the PL performance of AISe QDs via conventional direct synthesis. Herein, we develop the unique low-temperature (75 ℃) template-based synthesis of highly efficient near-infrared (NIR) luminescent AISe QDs from In₂Se₃ QDs via a facile cation exchange method. The brief synthesis AISe QDs process was as follows: firstly, indium acetate was dissolved in non-coordinating solvent octadecene. Selenium precursor was injected into the above mixture at 200 ℃, followed by nucleation and growth within a few minutes. Thereafter, In₂Se₃ template QDs can be acquired, and the dispersity of the as-prepared QDs can be improved by adding zinc. Secondly, silver acetate was added to the In₂Se₃:Zn²⁺ QDs solution with stirring for 15 min at 75 ℃. Finally, AgInSe₂:Zn²⁺ QDs were obtained. The proposed method enables the as-prepared AISe QDs to inherit the size and morphology of the template QDs. The extent of cation exchange can be controlled by rationally manipulating the Ag/In precursor molar ratio. We successfully regulate the stoichiometry of Ag/In ratio from 0.26 to 1.09. As a result, highly efficient luminescence of AISe QDs with the maximum absolute quantum yield of 42.5% has been achieved, which is higher than that of the AISe counterparts synthesized via the direct method. Moreover, we survey the luminescence mechanism of AISe QDs by means of the steady-state, transient and temperature-dependent spectroscopies. AISe nanoprobes were prepared by coating the hydrophobic QDs with a layer of 1,2-distearoyl-sn-glycero-3-phosphoethanol-amine-N-[biotin(polyethyleneglycol)- 2000] (DSPE-PEG-Biotin) phospholipids through hydrophobic interaction. By virtue of the excellent biocompatibility and intense NIR emission, we exemplify the application of AISe nanoprobes in the targeted cancer cell imaging, thus revealing their promising bioapplications including disease diagnosis and imaging-guided surgery.

Key words: AgInSe₂, near-infrared, quantum dots, cation exchange, luminescent nanoprobes

引用此文

廉纬, 方泽铠, 涂大涛, 李嘉尧, 韩思远, 李仁富, 商晓颖, 陈学元. 模板法控制合成AgInSe₂:Zn²⁺近红外荧光量子点及其生物标记应用^※[J]. 化学学报, 2022, 80(5): 625-632.

Wei Lian, Zekai Fang, Datao Tu, Jiayao Li, Siyuan Han, Renfu Li, Xiaoying Shang, Xueyuan Chen. Template-Based Controlled Synthesis and Bioapplication of AgInSe₂:Zn²⁺ Near-Infrared Luminescent Quantum Dots^※[J]. Acta Chimica Sinica, 2022, 80(5): 625-632.

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图/表 6

图1. 不同Zn/In投料物质的量比: (a1) 0, (a2) 0.2, (a3) 0.4, (a4) 0.6和(a5) 0.8所合成的In2Se3:Zn2+量子点的透射电镜明场像; 以及Ag/In投料物质的量比分别为(b1) 0, (b2) 0.3, (b3) 0.6, (b4) 0.9和(b5) 1.2所合成的AgInSe2:Zn2+量子点的透射电镜明场像. 插图为对应透射电镜明场像中随机挑选100个颗粒所得粒径统计图

Figure 1. (a) Transmission electron microscopy (TEM) images of In2Se3:Zn2+ QDs with precursor ratios of Zn/In of (a1) 0, (a2) 0.2, (a3) 0.4, (a4) 0.6 and (a5) 0.8, respectively; (b) TEM images of AgInSe2:Zn2+ QDs with precursor ratios of Ag/In of (b1) 0, (b2) 0.3, (b3) 0.6, (b4) 0.9 and (b5) 1.2, respectively. Insets show their corresponding size distribution histogram by randomly calculating 100 particles in the TEM images

图2. (a) In2Se3:Zn2+和(b) AgInSe2:Zn2+量子点的X射线光电子能谱全谱图; 不同Ag/In投料物质的量比所合成的AgInSe2:Zn2+量子点的(c) Ag 3d和(d) In 3d的X射线光电子能谱图

Figure 2. XPS analyses of (a) In2Se3:Zn2+ and (b) AgInSe2:Zn2+ QDs. XPS scans on (c) Ag 3d and (d) In 3d of AgInSe2:Zn2+ QDs with different precursor molar ratio of Ag/In

图3. 不同Zn/In投料物质的量比所合成的In2Se3:Zn2+量子点的(a)吸收光谱, (b)发射光谱(λex=365 nm)以及(c)荧光衰减谱图(375 nm激发下监测发射峰信号); 不同Ag/In投料物质的量比所合成的AgInSe2:Zn2+量子点的(d)吸收光谱, (e)发射光谱(λex=365 nm)和(f)荧光衰减谱图(375 nm激发下监测发射峰信号). 插图为相应量子点环己烷溶液实物图

Figure 3. (a) Absorption spectra, (b) PL emission spectra (λex=365 nm), and (c) PL decays upon excitation at 375 nm by monitoring the peak emission of In2Se3:Zn2+ QDs with different precursor molar ratio of Zn/In. (d) Absorption spectra, (e) PL emission spectra (λex=365 nm), and (f) PL decays upon excitation at 375 nm by monitoring the peak emission of AgInSe2:Zn2+ QDs with different precursor molar ratio of Ag/In. Insets show their corresponding photographs of QDs dispersed in cyclohexane solution

图4. In2Se3:Zn2+量子点的(a)变温发射光谱(λex=365 nm)和(b)发光强度随温度变化关系图; (c) AgInSe2:Zn2+量子点的变温发射光谱(λex=365 nm)和(d)发光强度随温度变化关系图, (e)不同Ag/In组分AgInSe2:Zn2+量子点发光机制示意图

Figure 4. (a) Temperature-dependent emission spectra of the In2Se3:Zn2+ QDs upon excitation at 365 nm, (b) PL intensities as a function of temperature in (a). (c) Temperature-dependent emission spectra of the AgInSe2:Zn2+ QDs upon excitation at 365 nm, (d) PL intensities as a function of temperature in (c). (e) Schematic illustration showing the proposed PL process in AgInSe2:Zn2+ with different stoichiometry of Ag/In

图5. (a) AgInSe2:Zn2+量子点表面修饰DSPE-PEG-Biotin示意图, 以及OA-QDs和Biotin-QDs分散在己烷与水的混合溶剂中的实物图照片; (b) OA-QDs和Biotin-QDs的傅里叶红外光谱图; Biotin-QDs在 pH=7.1水溶液中的(c) Zeta电势和(d)水合粒径统计图

Figure 5. (a) Schematic illustration of biotinylation of AgInSe2:Zn2+ QDs and photographs of OA-QDs and Biotin-QDs dispersed in hexane and water mixed solvent, respectively. (b) Fourier-transform infrared spectra of the OA-QDs and Biotin-QDs, (c) Zeta-potential and (d) hydrodynamic diameter distribution of Biotin-QDs dispersed in aqueous solution (pH 7.1)

图6. (a) Biotin-QDs探针靶向细胞成像示意图, Biotin-QDs探针分别和(b) HeLa细胞, 以及(c) L-02细胞孵育2 h后的共聚焦显微镜成像. 1至4列分别为明场像、408 nm激发下的4,6-二脒基-2-苯基吲哚(DAPI)染色细胞核像、量子点荧光像以及叠加图像

Figure 6. (a) Schematic illustration of targeted cell imaging based on Biotin-QDs nanoprobe. Confocal laser scanning microscopy images of Biotin-QDs incubated with (b) HeLa cells and (c) L-02 cells after 2 h. Panel 1 is the bright-field images. DAPI stained cell nucleus images (λex=408 nm) that indicate the nuclear regions are shown in panel 2. Panel 3 is the PL images (λex=408 nm) of QDs, and panel 4 is the overlay images of panels 1, 2 and 3

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模板法控制合成AgInSe₂:Zn²⁺近红外荧光量子点及其生物标记应用^※

Template-Based Controlled Synthesis and Bioapplication of AgInSe₂:Zn²⁺ Near-Infrared Luminescent Quantum Dots^※

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