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24 protocols using lambda 35 spectrometer

1

Synthesis and Characterization of Ru Complexes

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All manipulations were carried out
at room temperature under argon using standard Schlenk, high vacuum,
and glovebox techniques using dry and degassed solvents. C6D6, C6D5CD3, and THF-d8 were vacuum transferred from potassium. NMR
spectra were recorded at 298 K (unless otherwise stated) on Bruker
Avance 400 and 500 MHz NMR spectrometers and referenced as follows:
C6D6 (1H, δ 7.16; 13C, δ 128.0), C6D5CD3 (1H, δ 2.09), THF-d8 (1H, δ 3.58; 13C, δ 25.3). 31P{1H} spectra were referenced externally to 85% H3PO4 and 119Sn to SnMe4. IR
spectra were recorded on a Nicolet Nexus spectrometer and UV–vis
spectra on a PerkinElmer Lambda 35 spectrometer. Elemental analyses
were performed by Elemental Microanalysis Ltd., Okehampton, Devon,
U.K. [Ru(PPh3)3HCl]·toluene,43 (link) [Ru(PPh3)(C6H4PPh2)2H][Li(THF)2] (1)4 and IMe4,44 (link) were
prepared according to literature methods. Prior to use, [Ru(PPh3)3HCl]·toluene was dried under high vacuum
and ground to a fine powder affording a material with ca. 1 molecule
of toluene per Ru (based on 1H NMR analysis). IMe4 was purified by sublimation. LiCH2TMS was used as a colorless
solid obtained upon cooling a commercial 1.0 M solution in pentane
at −32 °C, separating the resulting colorless crystals
by decantation in a glovebox and drying under vacuum. AlMe2Cl (1.0 M solution in hexane, Merck) and SnMe3Cl (Merck)
were used as received.
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2

Photophysical Properties of NBD Compounds

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UV–vis absorption spectra of NBDH, NBD-PD, SBA-NBDH, and SBA-NBD-PD, in solid state/powder, were performed with a Perkin Elmer Lambda 35 spectrometer equipped with an integrating sphere, using a spectral on as a certified reflectance standard, at a scanning speed of 60 nm/min and a slit of 4 nm. Fluorescence emission and excitation spectra of NBDH, NBD-PD, SBA-NBDH, and SBA-NBD-PD, in solid state/powder, were registered using the Jasco FP-6500 spectrofluorometer, equipped with EFA-383 epifluorescence attachment, at a scanning speed of 100 nm/min and an excitation wavelength of 450 nm.
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3

Spectroscopic characterization of probes

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The UV/Vis absorption spectra and fluorescence spectra were scanned on a Perkin Elmer LAMBDA 35 spectrometer (PerkinElmer, Waltham, MA, USA) and a Hitachi F-7000 (Hitachi, Tokyo, Japan) respectively. 1H NMR spectra were obtained on a Bruker (400 MHz) spectrometer (Bruker, Karlsruhe, Germany). The excitation and emission slits were 5 nm and the PTM voltage of the spectrometer were 400 V.
The absorption and fluorescence spectra of probe A and probe B were measured in methanol (MeOH), EtOH and DCM, dimethyl formamide (DMF), and dimethyl sulfoxide (DMSO) respectively.
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4

Characterization of PDAP Nanoparticles

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1H NMR spectra were detected with Bruker AMX‐600 NMR spectrometer (Bruker, Switzerland) at 600 MHz. FTIR spectra were recorded with Thermo Nicolet 8700 infrared spectrometer (Thermo Fisher, Waltham, MA) using KBr powder. UV–Vis and fluorescence spectra were detected by Lambda‐35 spectrometer (PerkinElmer, Inc., Shelton, CT) and LS‐55 fluorescence spectrometer (PerkinElmer, Inc., Shelton, CT), respectively. The morphology of PDAP NPs was observed by transmission electron microscopy (Hitachi, Japan), and the molecular weight of PDAP NPs was determined with a MALDI‐TOF mass spectrometer (Bruker, Billerica, MA). The HOMO–LUMO orbital energy levels were calculated at the B3LYP/6‐31G/LANL2DZ level using density functional theory (DFT) in Gaussian 03 software. The DFT‐based B3LYP/6‐31g(d) model is applicable to molecular systems with C, N, and O atoms.
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5

Characterization of Honeycomb Polymer Films

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1H NMR spectra were obtained using a JEOL JNM-ECA300 at 300 MHz with CDCl3. Gel permeation chromatography (GPC) was performed by a set of a Waters 515 HPLC pump. The surface pore structure and morphologies of the honeycomb films were detected by a field emission scanning electron microscopy (FE-SEM, 10 kV, SU-8010) with energy dispersive X-ray spectrometry (EDS, 15 kV). Film samples were pre-coated with platinum before observed. The elements on the films were determined by SEM-EDS. Membrane morphologies and structures were studied by transmission electronic microscope (TEM, 80 KV, JEM 2010). The chemical structures of the coated polymer films were characterized by attenuated total reflection-Fourier transform infrared spectra in the range of 600–4000 cm−1 (ATR-FTIR, Bruker VERTEX70). The films were pre-treated in oven at 80 °C all-night before use. UV-Vis spectra were observed on PerkinElmer Lambda35 spectrometer.
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6

Comprehensive Characterization of Samples

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The morphology of the samples was observed on scanning electron microscopy (SEM) (Apreo S LoVac, FEI, Hillsboro, Oregon, USA) and transmission electron microscopy (TEM) (JEM-2100F, JEOL, Japan). The energy-dispersive X-ray spectroscopy (EDS) was used to analyze the element distribution in samples. The zeta potential of samples was measured on a Malvern Zetasizer instrument (Nano ZS, Malvern Instruments, Malvern, UK). X-ray diffraction (XRD) patterns were recorded on a D8 advance X-ray powder diffractometer (Burker, Germany) with a 2θ angle in the range of 10–50° to investigate the crystal structure of all samples. Fourier transform infrared (FT-IR) spectra were measured in the 4000–500 cm−1 on an FT-IR spectrometer (Nicolet AVATAR 360, Madison, Wisconsin, USA). The UV-vis-NIR spectra were recorded on a Lambda 35 spectrometer (Perkin Elmer, Waltham, Massachusetts, USA). Nitrogen adsorption/desorption isotherms were measured with ASAP 2420 (Micromeritics, Norcross, Georgia, USA). The specific surface area and pore size distribution of samples were calculated based on the Brunauer–Emmett–Teller (BET) method and the Barret–Joyner–Hallenda model, respectively [39 (link)].
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7

Metabolite Characterization by Mass Spectrometry

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Samples were dissolved in methanol, and electrospray ionization ion trap multiple mass spectrometry (ESI–MS) was performed on a MicrOTOF-Q II (Bruker Daltonics, Germany) plus LC/MS system. UV spectra were obtained using a Perkin-Elmer Lambda 35 spectrometer. 1H NMR spectra,13C NMR spectra,and 2D NMR (HMBC) spectra were recorded on a Bruker Ascend-400 spectrometer, operating at 400 and 100 MHz for 1H and 13C, respectively, using MeOD-d4 as solvents. Chemical shifts were reported in δ (ppm) downfield from tetramethylsilane (TMS) as an internal reference, and coupling constants were reported in Hz. Column chromatography (CC) was performed using silica gel (200–300 mesh, 2.4 kg) and Sephadex LH-20. The spots on TLC plates were detected under UV light or by holding under iode vapor, and were visualized by spraying with ethanol-H2SO4 after heating. Separations by HPLC (LC-3000) were carried out using an Welchrom-C18 column (10 × 250 mm, 5 μm).Unless specified otherwise,the flow rate was 2.0 mL/min.
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8

Spectroscopic Characterization of Samples

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Absorption measurements were recorded with a Lambda 35 spectrometer (PerkinElmer, Waltham, MA, USA) using 1 cm optical path quartz cuvettes. Fluorescence measurements were conducted with LS55B spectrofluorometer (PerkinElmer, Waltham, MA, USA) equipped with polarizers, thermostated cuvette compartments, and magnetic stirring. Induced circular dichroism spectra were registered by Chirascan-plus qCD (Applied Photophysics Limited, Surrey, UK), which was equipped with thermostat. All spectroscopic measurements were carried out at a room temperature (23–25 °C). Optical density of all samples did not exceed 0.4 a.u. All of the measurements were performed in triplicate.
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9

Prodigiosin Loading and Release from Halloysite

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The red pigment prodigiosin was obtained by cultivation of the producer strain S. marcescens ATCC 9986 on agarized peptone–glycerol medium. Pigment purification was performed as described previously (Guryanov et al., 2013 (link)). Ethanol solution (96% vol. 300 μl of purified prodigiosin (4.4 μg) was mixed with glycerol (70 μL), dry HNTs (30 mg) in centrifuge tube and placed into desiccator for loading by vacuum displacement (Supplementary Figure S1). Prodigiosin loading procedure was performed for 24 h. Subsequently, the loading efficiency was evaluated by thermogravimetric analysis (TGA) while Fourier transform infrared spectroscopy (FT-IR) highlighted the interaction mechanism and involved functional groups. Optical absorption spectra of purified prodigiosin in ethanol and extracts of glycerol-HNTs and prodigiosin-HNTs after 30 min and 2 h exposure in PBS were obtained and compared for estimation of pigment release from loaded halloysite nanotubes. Absorption spectra were analyzed using a Lambda 35 spectrometer (PerkinElmer).
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10

Fluorescence Characterization of mTHPC

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Absorption measurements were recorded with a Lambda 35 spectrometer (Perkin Elmer, USA) using integrating sphere and fluorescence measurements were conducted with LS55B spectrofluorometer (PerkinElmer, USA) equipped with polarizers, thermostated cuvette compartments and magnetic stirring for polarization experiments. Fluorescence quantum yield and photoinduced fluorescence quenching (PIQ) were measured as was previously described (λexc: 416 nm; λem: 652 nm) (Reshetov et al., 2011 (link)). mTHPC fluorescence polarization was performed as described earlier (Reshetov et al., 2011 (link)). Samples were excited at 435 nm and fluorescence was registered at 652 nm.
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