X ray diffractometer

Different other instruments such as Fourier transform infrared spectrometer [FTIR; JASCO (FT-4100), Tokyo, Japan], field emission transmission electron microscopy (FE-TEM; JEM-F200, JEOL, Japan), and X-Ray Diffractometer [XRD; X-Ray Diffractometer, Rigaku (Japan), Ultima IV] were used to determine the surface chemistry, morphology, and crystalline nature of Lam-AuNPs. A particle analyzer (Litesizer 500; Anton Paar, GmbH) was used to measure Lam-AuNP size and zeta potential. The same FE-TEM apparatus was used to analyze Lam-AuNPs energy dispersive spectroscopy (EDS).

XRD analysis of the AAS-loaded lipid nanoparticles (lyophilized in advance using mannitol 10%, w/v as the cryoprotectant) was performed using an X-ray diffractometer (Rigaku Corporation, Tokyo, Japan) to assess their crystalline structures. The X-ray diffraction patterns were recorded at 2θ values of 3–50° at a scanning speed of 5° per min using a Cu-Kα radiation source.

The DMNs were measured with an X-ray diffractometer (Rigaku, Japan) using Cu Kα radiation at a tube voltage of 40 kV, a current of 40 mA, and a scan 2θ angle range of 3 ~ 40°. The scanning speed was set at 0.1s/step with a step size of 0.02°. The DMNs samples to be tested were sprayed conductive coating and imaged using a scanning electron microscope (SEM, LEO 1530VP, Germany) equipped with an energy-dispersive X-ray spectroscopy (EDS, Germany). The DMNs were also cut into single rows and taken images using a fluorescence inverted microscope (IX73, Olympus, Japan). The mechanical property was tested by a pressure tester (Mark-10, USA), a cylindrical probe with a diameter of 10 mm compressed the microneedle arrays at a rate of 10.5 mm/min, and the force-displacement of the arrays was recorded to plotted the force-distance curve. The dynamic processes of Ef/CBD-SD@DMNs dissolving in different mediums were recorded by a fluorescence inverted microscope (IX73, Olympus, Japan).

The FT-IR spectra of organic compounds and polymers were recorded using Nicolet spectrometer. ¹ H NMR (400 MHz) and ¹³ C NMR (100 MHz) spectra were obtained with a Bruker Advance spectrometer at 25°C using CDCl₃ and DMSO- d₆ as solvent. Polyamides inherent viscosities were obtained with a polyamide concentration of 0.5 g/dL in DMF solvent at 30°C using an Ubbelhode suspended level viscometer. Differential scanning calorimetry (DSC) was measured on a Mettler Toledo DSC STAR ^e instrument at heating rate of 20°C/min. under nitrogen. The glass transition temperatures (T_g) were determined from DSC curves. Thermogravimetric analysis (TGA) was performed on a Mettler Toledo STAR ^e instrument at a heating rate of 10°C/min under nitrogen. Wide angle X-ray diffraction (WAXD) was measured with a Rigaku X-ray diffractometer using polyamide powder.

The crystalline phase of the synthesized particles was analyzed by Rigaku X-ray diffractometer (XRD, Tokyo, Japan) with Cu Kα radiation in the scan range of 10–90°. The morphology of particles in powder form and as coatings were investigated using the FEI Nova NanoSEM 650 field emission scanning electron microscope (FESEM) coupled with an energy dispersive spectroscopy (EDS) (TEAM™ Integrated EDS with Apollo X SDD) for X-ray microanalysis was used to determine the chemical composition of the samples. Samples were fixed on an aluminum stub with vacuum-resistant carbon tape. FESEM analysis was performed using a low-vacuum mode. An acceleration voltage of 15 kV and a working distance of around 5 mm was typically used.

Morphologies and structures of the AFeC FANDs were measured using the HT-7700 TEM (Hitachi, Janpan) and SU8010 SEM (Hitachi, Janpan). Zeta potential was characterized by DLS (Malvern, UK). EDS pattern was measured by the X-Ray Diffractometer (smartLab SE, Rigaku, Japan). UV-vis absorption feature and fluorescent spectrum were investigated by the UV-1800 spectrophotometer or the SpectraMaxM2/M2e Multi-mode Plate Readers (Molecular Devices, U.S.). Molecular dynamics (MD) simulation was performed by the GROMACS (2019.6) program. The drug loading content (DLC) and drug loading efficiency (DLE) of ALA, Cur, and iron ions in the AFeC FANDs or FeC FANDs were tested using HPLC (1260, Agilent, U.S.), the UV-1800 spectrophotometer, and 1,10-phenanthroline-based UV-vis approach^[1], respectively. $\mathrm{DLC}=\frac{weightofloadedALA}{weightofAF\mathrm{e}CFANDs}\times 100\%$ $\mathrm{DLE}=\frac{weightofloadedALA}{weightoftotalALAapplied}\times 100\%$