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Lcmsd trap xct spectrometer

Manufactured by Agilent Technologies

The LCMSD Trap XCT spectrometer is a laboratory instrument designed for high-performance liquid chromatography (HPLC) and mass spectrometry (MS) analysis. It combines a linear ion trap with an Orbitrap mass analyzer to provide accurate and sensitive mass detection. The instrument is capable of performing tandem mass spectrometry (MS/MS) experiments for structural elucidation and quantitative analysis of a wide range of analytes.

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3 protocols using lcmsd trap xct spectrometer

1

Analytical Techniques for Compound Characterization

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Optical rotations were measured on a PerkineElmer 341 polarimeter. 1H and 13C NMR spectra were recorded on Bruker Avance-500 spectrometers. ESI–MS were measured on an Agilent LC/MSD Trap XCT spectrometer, and HRESIMS were performed on an Agilent 6520 Accurate-MS Q-TOF LC/MS system. A preparative column (ZORBAX-ODS GSA10250AP1301, C18, 5 μm, 250 × 10 mm) was used for semi-preparative HPLC (Shimadzu LC-2010A HT). TLC analysis was run on HSGF254 silica gel plates (10–40 μm, Yantai, China). Column chromatography (CC) was performed on silica (100–200, 200–300 mesh, Yantai, China), YMC-GEL ODS-A (50 μm, YMC, Japan), Sephadex LH-20 (Amersham Pharmacia Biotech AB, Uppsala, Sweden).
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2

Synthesis and Characterization of Newkome-type Dendrimers

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Example 1

All chemicals were purchased from Sigma-Aldrich, Acros Organics, Alfa Aesar, Dendritech, or TCI international and used as received unless otherwise noted. Second generation Newkome-type dendrimer, aminononaester, succinate nonaester, and first generation Newkome-type acid dendrimer were synthesized as previously reported (Newkome et al., Chem. Rev. 110:6338-42 (2010), which is hereby incorporated by reference in its entirety) from starting materials purchased from Frontier Scientific. Dialysis membranes (SpectraPor 6) were purchased from Spectrum Labs and used after rinsing the membrane in water for 30 minutes. LC-MS data were recorded on an Agilent LCMSD Trap XCT spectrometer using electrospray ionization (ESI) and methanol as eluent for starting compounds and acetonitrile (0.1% TFA) for species purified by HPLC. 1H NMR spectra were recorded using a Bruker AV-400, -500, or -600 spectrometer (operating at 400.1 MHz, 500.2 MHz, or 600.2 MHz respectively). Chemical shifts are reported in ppm and the residual signals of the Deuterated solvents were used as references. 13C NMR spectra were recorded on a Bruker AV-400 spectrometer (100 MHz). Deuterated solvents were purchased from Cambridge Isotope Laboratories.

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3

Synthesis and Purification of Dendron Compounds

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All chemicals were purchased from Sigma-Aldrich, Acros Organics, Alfa Aesar, or TCI international, and used as received, unless otherwise noted. Dendrons 1 and 6 were synthesized as previously reported from starting materials purchased from Frontier Scientific. 3-Azidopropylamine was synthesized as previously reported. Dialysis membranes (SpectraPor 6) were purchased from Spectrum Labs and used after rinsing the membrane in water for 30 min. LCMS data were recorded on an Agilent LCMSD Trap XCT spectrometer using electrospray ionization (ESI) and methanol as eluent for starting compounds and acetonitrile (0.1% TFA) for species purified by HPLC. 1HNMR spectra were recorded using a Bruker AV-400, -500, or -600 spectrometer (400.1 MHz, 500.2 MHz, or 600.2 MHz); 13CNMR spectra were recorded on a Bruker AV-600 spectrometer (150.9 MHz). Deuterated solvents were purchased from Cambridge Isotope Laboratories. High-performance liquid chromatography (HPLC) purifications were run on a LC-8A Shimadzu (Kyoto, Japan) system equipped with a SPD-10Avp UV/Vis detector with reverse-phase Jupiter 10u C4 300A column (10 × 250 mm) in varying percentages of water and acetonitrile with 0.1% TFA at a rate of 5 mL/min.
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