The NMR spectra were recorded on an Agilent 400 MR spectrometer (Agilent, Santa Clara, CA, USA) operating at 400.445 MHz (1H). The Raman spectra were obtained using an Avantes AvaSpec-ULS-RS-TEC spectrometer with 788 nm laser excitation. Zinc-65 and gallium-68 were quantified by gamma spectroscopy using a Princeton Gammatech LGC 5 or Ortec GMX 35195-P germanium detector, calibrated using certified barium-133 and europium-152 sources. Zinc at natural abundance was quantified using a Thermo Scientific iCAP 6000 Series ICP Optical Emission Spectrometer. An Eppendorf 5702 centrifuge was used to assist in phase separation. All experiments used 0.2 µm membrane pore size, a 0.002” (0.051 mm) diaphragm, two 10-element static mixers, and a 108 cm mixing tube. The solutions for the continuous membrane-based separation were pumped using KDS 100 Legacy Syringe pumps. For batch experiments, phase mixing was performed using an IKA ROCKER 3D digital shaker.
Agilent 400 mr spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The Agilent 400 MR spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical applications. It provides high-resolution spectroscopic data on the molecular structure of chemical compounds.
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Lab products found in correlation
Centrifuge 5702, by Eppendorf (1 mentions)
Nicolet is5 ftir spectrometer, by Thermo Fisher Scientific (1 mentions)
Lcms it tof instrument, by Shimadzu (1 mentions)
Microtof q mass spectrometer, by Bruker (1 mentions)
C11347 quantaurus qy, by Hamamatsu Photonics (1 mentions)
Tcs sp5 2, by Leica camera (1 mentions)
Microtof q 2, by Bruker (1 mentions)
Silica gel 60 f254 plate, by Merck Group (1 mentions)
Miracle 10, by Shimadzu (1 mentions)
5 protocols using agilent 400 mr spectrometer
1
Quantification of Isotopes via Spectroscopy and Separation
2
Spectroscopic Characterization of Compounds
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IR spectra in the solid state were recorded on a Nicolet iS5 FTIR spectrometer (Thermo Fisher Scientific, Waltham, MA, USA) using an internal reflectance attachment with diamond optical element−attenuated total reflection (ATR) with a 45° angle of incidence. The resolution was 4 cm−1; the number of scans was 32. The NMR spectra were recorded in the standard 5 mm sample tubes using an Agilent 400-MR spectrometer (Agilent Technologies, Santa Clara, CA, USA) with operating frequencies of 400.1 MHz (1H), and 100.6 MHz (13C). Registration of HRMS ESI mass spectra was carried out using an LCMS-IT-TOF instrument (Shimadzu, Japan).
3
Characterization of Fluorescent Probes
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1H NMR and 13C NMR spectra were measured on an Agilent 400 MR spectrometer, and the chemical shifts were expressed in ppm and coupling constants (J) in hertz. High-resolution mass spectra (HRMS) were measured using a Bruker micrOTOF-Q mass spectrometer (Bruker Daltonik, Bremen, Germany). Fluorescence measurements were carried out on a Sancho 970-CRT spectrofluorometer (Shanghai, China). UV-vis absorption spectra were measured with a SP-1900 spectrophotometer (Shanghai Spectrum Instruments Co., Ltd., China). pH measurements were made with a Model PHS-25 Bmeter (Shanghai, China). Cell imaging was observed under a confocal laser scanning microscope (LEICA TCS SP5 II, Germany) with excitation at 405 nm. Fluorescence quantum yields were measured with an absolute fluorescence quantum yield spectrometer (Quantaurus-QY C11347, Hamamatsu Photonics).
Unless otherwise noted, reagents were purchased from commercial suppliers and used without further purification. 3 was prepared according to the reported method42 (link) (ESI† ). MCF-7 (human breast carcinoma) cells were obtained from Institute of Basic Medical Sciences (IBMS) of Chinese Academy of Medical Sciences (CAMS).
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1H NMR and 13C NMR spectra were measured on an Agilent 400 MR spectrometer, and the chemical shifts were expressed in ppm and coupling constants (J) in hertz. High-resolution mass spectra (HRMS) were measured using a Bruker micrOTOF-Q mass spectrometer (Bruker Daltonik, Bremen, Germany). Fluorescence measurements were carried out on a Sancho 970-CRT spectrofluorometer (Shanghai, China). UV-vis absorption spectra were measured with a SP-1900 spectrophotometer (Shanghai Spectrum Instruments Co., Ltd., China). pH measurements were made with a Model PHS-25 Bmeter (Shanghai, China). Cell imaging was observed under a confocal laser scanning microscope (LEICA TCS SP5 II, Germany) with excitation at 405 nm. Fluorescence quantum yields were measured with an absolute fluorescence quantum yield spectrometer (Quantaurus-QY C11347, Hamamatsu Photonics).
Unless otherwise noted, reagents were purchased from commercial suppliers and used without further purification. 3 was prepared according to the reported method42 (link) (ESI
4
NMR Spectroscopy Protocol for Chemical Analysis
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Each 1HNMR spectrum was performed on an Agilent 400 MR spectrometer (400 MHz for 1H, Agilent Technology, Santa Clara, CA, USA). The acquisition parameters are as follows: probe, 5 mm OneNMR probe; temperature, 298 K; pulse program, PRESAT solvent suppression; number of scans, 64; data points, 64 K; spectral width, 4800 Hz; relaxation delay (d1), 2 s; acquisition time, 3.408 s. All NMR spectra were processed with MestReNova software (version 12.0.1, Mestrelabs Research SL, Santiago de Compostella, Spain).The processing parameters are as follows: window function, exponential; line-broadening, 0.3 Hz. The phase and baseline were corrected manually. The chemical shifts were calibrated with solvent(CD3OD at δ 3.31).
5
Optimized Organic Synthesis Protocol
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Unless otherwise noted, moisture sensitive reactions were conducted under dry nitrogen. CH2Cl2 was distilled over CaH2. THF was distilled over sodium/benzophenone. Et2O and toluene were dried over molecular sieves 4. Thin layer chromatography (tlc): Silica gel 60 F254 plates (Merck). Flash chromatography (fc): Silica gel 60, 40–64 μm (Merck); parentheses include: diameter of the column (d), length of the stationary phase (l), fraction size (V), eluent. Melting point: Melting point apparatus Mettler Toledo MP50 Melting Point System, uncorrected. MS: microTOF−Q II (Bruker Daltonics); APCI, atmospheric pressure chemical ionization. IR: FT‐IR spectrophotometer MIRacle 10 (Shimadzu) equipped with ATR technique. Nuclear magnetic resonance (NMR) spectra were recorded on Agilent 600‐MR (600 MHz for 1H, 151 MHz for 13C) or Agilent 400‐MR spectrometer (400 MHz for 1H, 101 MHz for 13C); δ in ppm related to tetramethylsilane and measured referring to CHCl3 (δ=7.26 ppm (1H NMR) and δ=77.2 ppm (13C NMR)), CHD2OD (δ=3.31 ppm (1H NMR) and δ=49.0 ppm (13C NMR)) and DMSO‐d6 (δ=2.54 ppm (1H NMR) and δ=39.5 ppm (13C NMR)); coupling constants are given with 0.5 Hz resolution; the assignments of 13C and 1H NMR signals were supported by 2‐D NMR techniques where necessary.
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