Heteronuclear dual-metal atom catalysts for nanocatalytic tumor therapy

doi:10.1016/S1872-2067(22)64207-4

Abstract

Abstract:

Due to excellent catalytic activity and high atomic utilization rate, single atom catalysts (SACs) have become a rising star in the field of nanocatalytic medicine. Heteronuclear dual-atom catalysts (HDACs) retain the advantages of monoatomic catalysts, have more optionally regulated coordination environment, possess favorable synergistic effects between different active sites, and can break through the restriction of adsorption ratio of SACs, making them the most ideal candidates for catalytic tumor therapy. In this review, we first introduce the advanced characterization methods of HDACs. Then, HDACs in different application fields are classified and elaborated according to various preparation strategies. According to the pharmacodynamic mechanisms, the application of HDACs in the field of nanocatalytic tumor therapy is emphatically introduced. Finally, a concise but focused summary and perspective is provided to outline the current challenges and prospects for future development of HDACs for oncology therapy.

Key words: Heteronuclear, Dual-atom catalyst, Tumor therapy, Reactive oxygen, Fenton-like reaction

Jingyi Han, Jingqi Guan. Heteronuclear dual-metal atom catalysts for nanocatalytic tumor therapy[J]. Chinese Journal of Catalysis, 2023, 47: 1-31.

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Figures/Tables 22

Fig. 1. Schematic diagram of adsorption configurations for single and diatomic sites (blue: adsorbed molecules, such as O2 or N2).

Fig. 2. Characterization techniques for SACs.

Table 1 Main characterizations for analyzing DACs.

Method	Purpose	Advantage	Disadvantage	Ref.
Microscopy (TEM, HAADF-STEM)	Direct imaging of metal elements with atomic resolution is used to detect the size and distribution of metal single atoms. The technique also provides relevant local structural information of atomic-level sites on the supporting material.	(1) Since the principle is based on Rutherford scattering, the image is bright enough to allow the observation of thick samples and low contrast samples. (2) Using the strong excitation and high-resolution imaging of the objective lens during the scanning transmission mode, microdiffraction can be achieved, which enables the visual observation of single atoms with 3D structure fixed in the N-doped graphene framework.	(1) It can only provide regional imaging of a specified location, without the ability to observe a wide area. (2) Only the surface of the sample can be characterized, while the morphology and structure of the core material encapsulated in the shell materials with 3D structure cannot be observed.	[114, 128‒131]
XAFS	Used to characterize the local geometric or electronic structure of a sample. It can elucidate the physical distance, coordination state, electronic structure and other highly accurate local information in atomic level.	(1) The overall structure can be determined by accurate in situ characterization of the single bimetallic atoms. (2) It can provide information about the stable adsorption structure and chemical bonding state of single atom on substrate materials. (3) The oxidation state and coordination number of the metal center in the complex can be characterized.	(1) Because X-rays are destructive, they can damage samples during measurements. (2) For XANES, there is the effect of multiple scattering emitted by photoelectrons and Auger electrons. Therefore, it is difficult to determine the identity of the oxidation states and scattering atoms.	[132‒135]
FTIR	By monitoring the adsorption behavior of these highly responsive guest molecules, the dispersion status of atomic-level metal sites in functional carriers was evaluated.	(1) High sensitivity, samples even below 10 nanograms can obtain satisfactory FTIR spectrograms. (2) The sample preparation is simple, and the reflectance spectrum of the opaque sample can be measured directly. (3) In the process of analysis, the original morphology and crystal form of the sample can be maintained without any detriment of the sample.	The analysis of complex mixtures and aqueous solutions is complicated.	[136‒140]
Mössbauer spectroscopy	Used to detect the coordination structure and electronic properties of materials such as oxidation states, spin states, chemical bond properties and other microscopic structure information.	(1) Mössbauer spectroscopy has extremely high energy resolution. (2) Because the Mössbauer effect involves resonant transition, the energy level structure, which depends on the chemical environment of the nuclear determines the shape and spectrum parameters, so it can reflect the change of the chemical environment around the resonant nuclear extremely sensitively. (3) Mössbauer spectroscopy has very little damage to the sample. (4) The test objects can be crystalline, amorphous, powdery or even frozen solutions, and the range of applications is extremely wide.

Table 1 Main characterizations for analyzing DACs.

Method	Purpose	Advantage	Disadvantage	Ref.
Microscopy (TEM, HAADF-STEM)	Direct imaging of metal elements with atomic resolution is used to detect the size and distribution of metal single atoms. The technique also provides relevant local structural information of atomic-level sites on the supporting material.	(1) Since the principle is based on Rutherford scattering, the image is bright enough to allow the observation of thick samples and low contrast samples. (2) Using the strong excitation and high-resolution imaging of the objective lens during the scanning transmission mode, microdiffraction can be achieved, which enables the visual observation of single atoms with 3D structure fixed in the N-doped graphene framework.	(1) It can only provide regional imaging of a specified location, without the ability to observe a wide area. (2) Only the surface of the sample can be characterized, while the morphology and structure of the core material encapsulated in the shell materials with 3D structure cannot be observed.	[114, 128‒131]
XAFS	Used to characterize the local geometric or electronic structure of a sample. It can elucidate the physical distance, coordination state, electronic structure and other highly accurate local information in atomic level.	(1) The overall structure can be determined by accurate in situ characterization of the single bimetallic atoms. (2) It can provide information about the stable adsorption structure and chemical bonding state of single atom on substrate materials. (3) The oxidation state and coordination number of the metal center in the complex can be characterized.	(1) Because X-rays are destructive, they can damage samples during measurements. (2) For XANES, there is the effect of multiple scattering emitted by photoelectrons and Auger electrons. Therefore, it is difficult to determine the identity of the oxidation states and scattering atoms.	[132‒135]
FTIR	By monitoring the adsorption behavior of these highly responsive guest molecules, the dispersion status of atomic-level metal sites in functional carriers was evaluated.	(1) High sensitivity, samples even below 10 nanograms can obtain satisfactory FTIR spectrograms. (2) The sample preparation is simple, and the reflectance spectrum of the opaque sample can be measured directly. (3) In the process of analysis, the original morphology and crystal form of the sample can be maintained without any detriment of the sample.	The analysis of complex mixtures and aqueous solutions is complicated.	[136‒140]
Mössbauer spectroscopy	Used to detect the coordination structure and electronic properties of materials such as oxidation states, spin states, chemical bond properties and other microscopic structure information.	(1) Mössbauer spectroscopy has extremely high energy resolution. (2) Because the Mössbauer effect involves resonant transition, the energy level structure, which depends on the chemical environment of the nuclear determines the shape and spectrum parameters, so it can reflect the change of the chemical environment around the resonant nuclear extremely sensitively. (3) Mössbauer spectroscopy has very little damage to the sample. (4) The test objects can be crystalline, amorphous, powdery or even frozen solutions, and the range of applications is extremely wide.

Fig. 3. (a) Fe-Co dual-site structure. M?ssbauer spectra of Fe,Mn/N-C (b) and Fe,Mn/N-C (c) under room-temperature. (d) Al MAS-NMR spectra. (e) Intensity changes. (f) Photographs of Pt-Al2O3 samples under white light and UV light (365 nm). (a,b) Reproduced with permission [125]. Copyright 2017, American Chemical Society. (c) Reproduced with permission [126]. Copyright 2021, Springer Nature. (d?f) Reproduced with permission [148]. Copyright 2017, Springer Nature.

Fig. 4. Schematic diagrams of the mechanisms of typical high-temperature pyrolysis (a), wet chemical double-solvent (b), Pt ALD mechanism on graphene nanosheets (c) and soft template self-assembly methods (d). (a) Reproduced with permission [163]. Copyright 2021, Royal Society of Chemistry. (b) Reproduced with permission [155]. Copyright 2018, Royal Society of Chemistry. (c) Reproduced with permission [164]. Copyright 2022, Elsevier. (d) Reproduced with permission [165]. Copyright 2022, John Wiley and Sons Ltd.

Fig. 5. (a) Schematic diagram of various construction strategies of MOF-based SACs. HAADF-STEM image of Fe-Mn dual sites (b) and corresponding intensity profiles (c). (d) Fe M?ssbauer spectrum. Fe (e) and Mn (g) K-edge XANES spectra. Fe (f) and Mn (h) Fourier-transform EXAFS spectra. (i) WT of the k2-weighted EXAFS data. (a) Reproduced with permission [28]. Copyright 2020, Royal Society of Chemistry. (b?i) Reproduced with permission [186]. Copyright 2022, Elsevier.

Fig. 6. Schematic diagrams of the synthesis of (Fe,Co)/CNT (a) and the structure of Fe-Co sites (b). HAADF-STEM image (c) and the EELS (d) of the (Fe,Co)/CNT. Various intermediate geometric structures (e) and ORR free energy diagram (dashed line: the traditional 2e? pathway) (f) on (Fe,Co)/CNT. (g) Relationship between ORR activity and ΔGOH*. Co-SAs: Co site of bare Co SAs/N-C). Synthetic illustration (h) and HAADF images (i,j) of A-CoPt-NC. (k) Bimetallic atomic configuration model derived from the (h) region. (l?q) Theoretical calculation results of A-CoPt-NC. (l) ORR free energy diagram of (Co-Pt)@N8V4. Local state densities (m,n) and charge density vertical views (o,p) of (Co-Pt) @N8V4 (m,o) and (Pt-Pt)@N8V4 (n, p). (q) ORR pathway on (Co-Pt)@N8V4. (a?g) Reproduced with permission [187]. Copyright 2018, Royal Society of Chemistry. (h?q) Reproduced with permission [188]. Copyright 2018, American Chemical Society.

Fig. 7. Synthetic illustration of CoPNi-N/C (a) and CoDNi-N/C (b). Change of Bader charge in Co-N/C (c) and Co/Ni-N/C (d). Average electron density difference in plane between Co-N/C (e) and CoXNi-N/C (f) (yellow regions: the electron accumulation, cyan regions: the electron depletion). (g) Synthetic illustration of (Fe,Co)/NC. (h) HAADF-STEM images of (Fe,Co)/N-C (red circles: Fe/Co bimetallic active site). (i) Intensity profiles of corresponding zoomed areas in (h). (j) HRTEM image; XANES spectra (k) of (Fe,Co)/N-C and corresponding Fe EXAFS fitting data (l). (m) The structure of Fe-Co dual sites. (n) ORR intermediate and transition state energies of (Fe,Co)/N-C. (a?f) Reproduced with permission [198]. Copyright 2019, Elsevier. (g?n) Reproduced with permission [125] Copyright 2017, American Chemical Society.

Fig. 8. XANES spectra of Co K-edge (a) and Zn K-edge (c). (b,d) FT EXAFS spectra of corresponding samples. (e) Optimized calculated geometry of the Zn/CoN-C. (f) Optimized adsorption configuration geometry of O2. (g) Possible ORR reaction pathways in acidic environments. (h,i) ORR free energy diagram. Synthetic illustration (j) and HAADF image (k) of (Zn, Co)/NSC. (l) Corresponding intensity profiles. (m) Optimized calculated geometry of the (Zn, Co)/NSC. (n) Optimized adsorption configuration geometry of O2. (o,p) ORR free energy diagrams. (a?i) Reproduced with permission [199] Copyright 2019, John Wiley and Sons Ltd. (j?p) Reproduced with permission [200]. Copyright 2019, Elsevier BV.

Fig. 9. (a) Schematic diagram of the ice-assisted photocatalytic reduction method. (b?j) The geometry structures of different samples. (k) PDOS plots. HAADF-STEM (l) and element maps (m?p) of PtRuSA-CN620. Ru K-edge (q) and Pt L3-edge XANES (r) and FT spectrum of Ru/Pt at (s,t) R and (u,v) k spaces. Reproduced with permission [201]. Copyright 2019, Royal Society of Chemistry.

Fig. 10. (a) Synthetic illustration. (b) HAADF-STEM image. EELS spectrum (c) and corresponding contrast profiles (d) and EELS mapping (e) of (Fe,Co)/N-C. (f) Schematic diagram of the synthesis. HAADF-STEM image (g) and contrast profiles (h) of IrCo-N-C. Charge density diagrams of CoN4 (i) and IrCoN5 (j). XANES spectra (k,l), FT-EXAFS spectra (m,n) and EXAFS fitting curves (o,p) at Co K-edge (k,m,o) and Ir L3-edge (l,n,p). Ir L3-edge WT images for Ir/C (q), Ir-N-C (r), and IrCo-N-C (s). PDOS diagrams of CoN4-O (t) and IrCoN5-O (u). (v) Schematic bond formation of the Co?O bond. (a?e) Reproduced with permission [207]. Copyright 2020, American Chemical Society. (f?v) Reproduced with permission [208]. Copyright 2021, American Chemical Society.

Fig. 11. (a) Schematic diagram of the synthesis of Fe-NiNC. TEM (b,c) and HAADF-STEM (d) images of Fe-NiNC. (e) The Fe-Ni distance measurements. (f,g) XANES spectra. (h,i) FT-EXAFS. Free energy diagrams (j,k) and proposed mechanisms (l,m) for ORR (j,l) and OER (k,m). (a?m) Reproduced with permission [209]. Copyright 2020, Elsevier BV.

Fig. 12. (a) Synthetic illustration of Pt-Ru dimers/NCNTs using ALD technology. (b) HAADF-STEM image. (c) The intensity profile. (d) Distribution histogram of various structure tapes. (e) The ratio of loading Pt and Ru atoms under different ALD temperatures; XANES spectra (f,g,i) and corresponding k2-weighted FT-EXAFS (h,j). (k) Most stable H adsorption configurations. (l) Surface models. (m) Most stable adsorption configurations of OH. (a?j) Reproduced with permission [217]. Copyright 2019, Springer Nature. (k?m) Reproduced with permission [218]. Copyright 2019, American Chemical Society.

Fig. 13. (a) Synthetic illustration of various catalysts. (b) Ligand release curve during the titration. (c) DRIFTS spectra. (d,e) STEM images of Pt-Sn nanocluster. (f,g) Obvious intensity differences between Pt and Sn along the directions of the lines marked in (e). (a?c) Reproduced with permission [219]. Copyright 2022, American Chemical Society. (d?g) Reproduced with permission [220]. Copyright 2022, Wiley-VCH Verlag GmbH & CO. KGaA.

Fig. 14. (a) Synthetic illustration of FeCo-NSC. AFM image and corresponding height profile (b) and HAADF-STEM image (c). (d) The intensity plots of Fe-Co sites. (e,h) XANES spectra. FT-EXAFS spectra (f,i) and corresponding fitting in R space (g,j) of Fe K-edge (e?g) and Co K-edge (h?j) of FeCo-NSC and related samples. (k,l) HAADF-STEM images of the CN-FeNi-P. (m,p) XANES profiles. (n,q) EXAFS spectra FT k3-weighted in R space. (o,r) WT images of Fe K-edge (m?o) and Ni K-edge (p?r) of CN-FeNi-P and related samples. (a?j) Reproduced with permission [221]. Copyright 2022, Elsevier. (k?r) Reproduced with permission [222]. Copyright 2022, Elsevier.

Fig. 15. Schematic diagram of biological consequences of ROS increase. Oncogenic signals in tumor cells stimulate increased ROS production. Endogenous ROS and exogenous DNA damage agents, mitochondrial mutations cause respiratory chain failure and further increase ROS production. The above fault may affect the apoptotic response to anticancer drugs, making cancer cells resistant to the drugs. A surge in cellular ROS causes DNA damage and promotes mutations, which in turn leads to increased drug sensitivity.

Fig. 16. Schematic diagrams of the mechanism of endogenous Fenton response triggered by MSFP (a) and follow-up anti-tumor therapy for MSFP (b). Growth (c) and survival curves (d) of mice 4T1 tumor. (e) Schematic diagram of MSFP catalyzing the formation of ?OH, resulting in the oxidation of TMB (colorless) to oxTMB (blue). (f) Normalized absorbance of MB (C/C0) after 30 min in acidic PBS containing 100 μm H2O2. (g) Michaelis-Menten dynamics. (h) Line Weaver-Burk plotting of MSFP. (a?h) Reproduced with permission [235]. Copyright 2022, John Wiley and Sons Ltd.

Fig. 17. (a?d) Schematic diagram of the synergistic and “division of labor” catalytic mechanisms of FeCo-DIA/NC for “ROS cycling” and concurrent catalytic therapy in tumors. (e?h) DFT simulations of Fenton activity. Proposed reaction mechanisms at the Fe (e) and Co (g) sites. Free energy diagrams of Fenton process at Fe (f) and Co (h) sites. (i) Schematic diagram of in vivo studies. Body weight curve (j), tumor tissue proliferation curve (k) and survival rate (l) of mice during treatments. (m) Digital photographs of the dissected tumor. Reproduced with permission [16]. Copyright 2022, Elsevier.

Fig. 18. (a) The structure of (Fe, Pt)SA-N-C. (b) Fe K-edge EXAFS. (c) Pt L3-edge EXAFS. (d,e) In vivo treatment options. Tumor growth curves (f), weight change curves (g), Photos (h) of corresponding tumor tissue. (i) ESR spectra of BMPO/?OH. (j) Probable Fenton-like reaction mechanisms for attaining ?OH on (Fe,Pt)SA-N-C. (k) H2O2 adsorption models. (l) Free energy diagrams for Fenton-like reaction. Projected density of states of (Fe, Pt)SA-N-C after adsorbing H2O* (m) and H2O2* (n). Reproduced with permission [236]. Copyright 2022, American Chemical Society.

Fig. 19. (a) Schematic diagram of the synthesis of RBC-HNTM-Pt@Au and the efficient treatment of osteomyelitis via SDT mechanism. (b) Photos of the rat surgical site. (c) Routine blood tests after 4 weeks of treatment (n = 3). (d) Photoluminescence spectra. (e) The 1O2 comparison curve detected by 1,3-diphenylisobenzofuran (DPBF) degradation. (f) Ultrasonic current test. (g) Electrochemical impedance spectra. Reproduced with permission [240]. Copyright 2021, American Chemical Society.

Fig. 20. Schematic diagrams of sonocatalytic mechanism (a) and osteomyelitis operation via sonodynamic therapy (b). Charge density difference (c,f) of g-ZnN4, bad charge, O2 activated energy, magnetic moment (d,g), and DOS (e,h) of g-ZnN4 (c?e) and g-ZnN4-MoS2 (f?h). (i) The infected leg wound. (j) Fluorescence intensity statistics of inducible nitric oxide synthase and transforming growth factor-β. (k) Micro-CT analysis of infected legs. Reproduced with permission [241]. Copyright 2022, Wiley-VCH Verlag.

Fig. 21. Schematic diagrams of the synthesis of samples (1?5) (a) and crystal structures of samples (3) and (5) (b). (c) Viability of normal Caco-2 cells treated with samples 1?5 for 72 h after 15 d of inoculation (n ≥ 12). Reproduced with permission [245]. Copyright 2022, MDPI AG.

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