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13 protocols using accutof jms t100lc

1

Synthesis and Analysis of β-Galactosidase Probes

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For synthetic protocols of β-galactosidase fluorescence probes, see the Supplementary Information. Preparative HPLC was performed on HPLC system composed of a pump (PU-2080, JASCO) and detector (MD-2015, JASCO), with an Inertsil ODS-4 (10.0 mm × 250 mm) column (GL Sciences, Inc.). NMR spectra were recorded on a JNM-LA300 instrument (JEOL) at 300 MHz for 1H NMR and 75 MHz for 13C NMR. Mass spectra were measured with a JMS-T100LC AccuToF (JEOL).
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2

Characterization of Polymers by FTIR and DART-MS

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Attenuated total reflection spectra in the range 4000–400 cm−1 of the polymers were measured with Fourier transform infrared (FTIR) spectroscopy (Nexus 8700, Thermo Nicolet, Madison, WI, USA) and Omnic software version number 9.1.26 (Thermo Fisher Scientific Inc., Waltham, MA, USA) and a uniform resolution of 2 cm−1 was maintained in case of polymers. Analysis was performed on a DART (IonSense, Inc. Saugus, MA, USA) ion source coupled to a JMS-T100LC AccuTOF™ (JEOL Inc., Peabody, MA, USA) mass spectrometer using modifications of a previously published method [14 (link)]. In brief, 2 mg/mL polyethylene glycol in methanol solution (PEG 600), was used for exact mass calibration. Calibration was done by dipping the sealed end of a capillary tube (Kimble Glass Company, Vineland, NJ, USA) in the PEG 600 calibration solution and “wanding” the capillary tube in the sample gap for a few seconds. JEOL MassCenter software version 1.3.4 m (JEOL Inc., Peabody, MA, USA) was used to gather and analyze the data. Each data file contained a calibration curve developed from the PEG 600 calibration standard and was subsequently applied to all polymer data collected.
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3

Characterization of Organic Compounds

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1H NMR spectra were recorded on a JNM-LA300 (JEOL) instrument (300 MHz for 1H NMR) or JNM-LA400 instrument (400 MHz for 1H NMR). Mass spectra (MS, ESI-TOF) were measured with a JMS-T100LC AccuTOF (JEOL). Absorption spectra were obtained with a UV-1650PC UV/Vis spectrometer (Shimadzu), and fluorescence spectra were obtained with a F4500 fluorescence spectrometer (Hitachi). LC-MS analysis were performed on a reverse-phase column (Inertsil C18, GL Sciences (Tokyo, Japan)), fitted on an Agilent Technologies 1200 series/6130 Quadrupole (LC/MS) system, using a linear gradient of eluent A (0.1% formic acid in H2O) and eluent B (0.1% formic acid in 80% acetonitrile, 20% H2O) (A/B: 95/5 to 5/95 in 17.5 min). Detected at 490 nm. All experiments were carried out at 298 K, unless otherwise specified.
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4

Characterization of Molecular Structures

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Electrospray ionization mass (ESI-MS) spectrometry was conducted with a JEOL JMS-T100LC AccuTOF. UV-vis absorption and photoluminescence spectra were recorded with a JASCO V-760 spectrometer and a JASCO FP-8500 spectrofluorometer, respectively. CD spectra were measured on a JASCO J-725 spectropolarimeter.
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5

MALDI-TOF and ESI-TOF Mass Spectrometry

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Mass spectra were measured on a matrix-assisted laser-desorption ionization–time-of-flight mass spectrometer (ultraflex MALDI-TOF/TOF, Bruker). The sample solution was mixed with 500 mM 2,5-dihydroxybenzoic acid in chloroform/methanol (1:1) solution as the matrix and dried on the plate. High resolution mass spectra were measured on a time-of-flight mass spectrometer JMS-T100LC AccuTOF (JEOL) equipped with an electrospray ionization source in the positive ion mode. The extracted samples were dissolved in methanol and applied to the mass spectrometer. The settings of the instrument were calibrated using sodium trifluoroacetate. The ion-source temperature was 250 °C. The mass analyzer was scanned from m/z 300 to 1500 for the full scan analysis.
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6

NMR and Mass Spectrometry Analysis

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Chemicals were purchased
from Wako Pure Chemical Industries, Ltd., and used as received without
further purification. 1H NMR and 19F NMR spectra
were measured with JEOL ECA (600 MHz). Mass spectra were measured
with mass spectrometers (JEOL AccuTOF JMS-T100LC for ESI and JMS-700
MStation for EI).
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7

JEOL AccuTOF DART+ Mass Spectrometry

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The mass spectrometer instrument was a JEOL AccuTOF: JMS-T100LC with ionization mode DART+.
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8

ESI-MS Analysis of Compounds

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High-resolution mass spectra (ESI-MS) were obtained using an Agilent 1100 HPLC coupled to a JEOL AccuTOF (JMS-T100LC) (Peabody, MA, USA). All isolated compounds were prepared in MeOH and injected directly into a 0.3 mL/min stream of either MeOH or 80% MeOH/20% DI H20. Twenty microliters of sample (approximately 0.1 mg/mL) were injected manually at 0.5 min while mass drift compensation standards [L-tryptophan (negative ion), PEG (positive ion)] were injected at 1.5 min over the course of a 2 min run.
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9

Comprehensive Chemical Characterization

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High-resolution mass spectra were recorded using a JEOL AccuTOF JMS T100LC instrument fitted with an electrospray ion source. The spectrum was recorded over the mass range 50–1000 m/z.
UV-Vis absorption spectra were recorded on-line during HPLC analysis over the wavelength range 240–600 nm in steps of 2 nm.
NMR samples were prepared by dissolving the isolated compounds in hexadeuterated dimethylsulfoxide (99.9 atom % D, Sigma-Aldrich). The 1D 1H and the 2D 1H-13C HMBC, 1H-13C HSQC, 2D 1H-1H COSY and 1H-1H ROESY NMR experiments were obtained at 600.13 MHz and 150.90 MHz for 1H and 13C, respectively, at 298K on a Bruker 600 MHz instrument equipped with a cryogenic probe.
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10

Spectroscopic Characterization of Compounds

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NMR spectra, including
bidimensional, were recorded in CD3OD, CDCl3, or DMSO-δ6 solution on a Bruker Avance III HD
or Bruker BioSpin (Billerica, MA) spectrometer at either 700 or 400
MHz (1H) and 175 or 100 MHz (13C), using TMS
as an internal standard. High-resolution mass spectra, HRMS (ESI-TOF+), were acquired with a JEOL AccuTOF JMS-T100LC (Peabody,
MA) spectrometer. Optical rotation was obtained with an Anton Paar
MCP 150 polarimeter. Gas chromatography–mass spectrometry (GC–MS)
determinations were made using an Agilent 5975C system equipped with
a 30 m DB-5MS capillary column (0.25 mm i.d.; 0.25 mm). Preparative
HPLC was carried out with a Waters instrument (Milford, MA) equipped
with a 2535 pump and a 2998 photodiode array detector, using an XBridge
Prep Shield RP-C18 (19.0 × 250 mm2, 5 mm particle
size) packed column, and different gradient systems of MeCN and 0.1%
aqueous formic acid, at a flow rate of 17.06 mL/min. Control of equipment,
data acquisition and processing, and management of chromatographic
information were performed using the Empower 3 software package. Column
chromatography (CC) was carried out on silica gel 60 (Merck, Darmstadt,
Germany) or Sephadex LH-20 (GE Healthcare, Little Chalfont, Buckinghamshire,
U.K.). Thin-layer chromatographic (TLC) analyses were performed on
silica gel 60 F254 plates (Merck) and visualized using a Ce2(SO4)3 (10%) solution in H2SO4.
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