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7 protocols using 6130 quadrupole ms

1

Characterization of Natural Products

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Optical rotations were measured on an A. Krüss Optronic P8000 polarimeter. The IR spectra were collected on a Perkin Elmer Spectrum One FTIR spectrometer. The HR-ESIMS spectra were recorded on a Waters LCT Premier XE mass spectrometer. The ESIMS spectra were recorded on an Agilent 1260 LC system equipped with a DAD detector and coupled to an Agilent 6130 Quadrupole MS with an ESI source. The NMR spectra were recorded on Bruker Avance III HD 500 or AV600 spectrometers. The ECD spectra were recorded on a Jasco J-810 spectropolarimeter with MeOH as solvent. Flash cartridge (Reveleris, HP-silica, 12 g, 20 µm), Kinetex C18 (Phenomenex, 2.6 µm, 2.1 × 100 mm), and semi-preparative C18 (Grace, 5 µm, 10 × 250 mm) were used. All solvents used for extraction were analytical grade, and solvents for HPLC were HPLC grade.
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2

Purification of β-Amyloid Peptides by Mass-Directed HPLC

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β-Amyloid peptides were purified using mass-directed HPLC on an Agilent 1260 Infinity HPLC system coupled to a 6130 quadrupole MS. Column - Agilent Zorbax 300 SB C3 9.4 × 250 mm, 5 μm, 300 Å semi-preparative column heated to 60 °C; flow rate 4 mL/minute; Solvent System - A = water with 0.1% TFA, B = acetonitrile with 0.1% TFA; Gradient − 3 minute hold at 1% B, 1–61% B gradient over 60 minutes, 3 minute hold at 61% B. Fractions were automatically collected at one-minute intervals. In addition to use of the intrinsic mass spectra generated by this approach, fractions were screened as above for RPFC.
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3

Spectroscopic Analysis of Molecular Compounds

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Specific rotations were obtained using a JASCO P-2000 polarimeter with a 1-cm cell at 25°C. UV spectra were obtained using an Applied Photophysics Chirascan™-plus spectrometer with a 1-cm quartz cell at 25°C. IR spectral data were obtained using a JASCO FT/IR-4200 spectrometer. NMR spectra were recorded on an 800 MHz Bunker Avance III HD spectrometer with a 5-mm TCI cryoprobe and a Bunker Avance 600 MHz spectrometer at the National Center for Inter-university Research Facilities (NCIRF). LC-MS and low-resolution electrospray ionization mass spectroscopic (LR-ESI-MS) data were obtained using an Agilent Technologies 1200 series high performance liquid chromatography (HPLC) coupled with an Agilent Technologies 6130 quadrupole MS. High-resolution fast atom bombardment MS (HR-FAB-MS) data were obtained using a JEOL JMS-700 high-resolution MS at NCIRF.
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4

Nicotine Quantification by LC-MS

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Nicotine concentrations were determined by LC-MS using the Agilent 1260 Infinity liquid chromatography system with 6130 quadrupole MS. Aliquots (20 μl) of each sample were injected into a Poroshell 120 EC-C8 column (4.6 mm by 50 mm, 2.7 μm; Agilent Technologies) and subjected to a gradient (A to B, where A = 0.1% formic acid in water and B = 0.1% formic acid in acetonitrile) of 0% B for 3 min, 0% B to 100% B from 3 to 7 min, and 100% B from 7 to 10 min at a constant flow rate of 0.5 ml/min. A column-solvent equilibration time of 3 min was implemented before the next sample was analyzed. The following were the MS operational parameters: API-ES (atmospheric pressure ionization electrospray) mode, channel 1 (90%) positive single ion monitoring of mass/charge ratios 166 (50%, nicotine D3) and 163 (50%, nicotine) and channel 2 (10%) scan for positive ions, nitrogen as a nebulizing and drying gas (35 psi, 12 L/min), high capillary voltage of 4 kV, and drying gas temperature to 300°C. To protect the detector from salts in the buffer, MS was turned on with a delay of 1.4 min after the injection.
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5

Peptide Analysis by LC-MS

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1 mg of peptides, which were dissolved in 1 mL of water, was analyzed using an Agilent 1260 Infinity LC equipped with an Agilent 6130 Quadrupole MS. An Agilent Zorbax SB-C18 4.6 Â 250 mm column was used together with a mixture of two different solutions of 0.1% (v/v) formic acid -water (A) and 0.1% (v/v) formic acid -acetonitrile (B). The flow of mobile phase was 1.5 mL min À1 with a composition of 98% A -2% B for the first 1 min. From 1 to 18 min, the flow of B increased until 98% B and turned back to 2% again. The LC chromatogram was obtained at a wavelength of 220 nm.
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6

Comprehensive Analysis of Seed Oil Composition

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The FTIR spectra were recorded by Shimadzu IR-Prestige spectrometer in thin-film transmittance technique in KBr cell with the scan resolution of 4.0 cm -1 in the range from 450 to 4000 cm -1 .
The UV spectra of seed oils in n-hexane were measured in quartz cells (1 cm) with a Shimadzu UV 1550 spectrophotometer.
The 1 H NMR 600 Hz and 13 C NMR 151 Hz spectra were recorded on a JNM-ECA spectrometer (JEOL KOREA LTD.) in CDCl 3 using TMS as an internal reference standard.
RP-HPLC Agilent 1260 Infinity coupled with a system with diode array (PDA) and mass spectrometric detectors (MS) ( 6130 Quadrupole MS, Agilent Technologies, US) and Shimadzu LC20 with refractive index detector (RID 10 А) were used for the analysis of TAGs and FAs, respectively.
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7

HPLC-MS Analysis of Triacylglycerols

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For the separation of TAGs, Shimadzu LC20 chromatographic system with refractive index detector (RID 10A) and an Agilent 1200 Infinity chromatograph system with diode array and MS detectors were used. Chromatograms were recorded using mobile phases of the systems “acetonitrile-propan-2-ol” and “acetone – acetonitrile” for refractive index (RI) and DAD detector, respectively. The speed of the mobile phase was 0.8 mL/min; chromatographic columns of 250 × 4.6 mm Kromasil 100-5C18 (for HPLC with spectrophotometric detection) and 150 × 2.1 mm Kromasil 100–5C18 (for MS detection) were used at a thermostat temperature of 30°C.
Mass spectrometric detection (6130 Quadrupole MS, Agilent) was carried out in the atmospheric pressure chemical ionization mode under standard conditions at a fragmentor voltage of 150 V; signals were recorded for positively charged ions. The Kromasil 110-3.5C18 2.1 × 150 mm column was used, the mobile phase speed was 0.1–0.2 mL/min, and the eluent system was acetonitrile– propanol-2 with additions of ammonium formate (HCOONH4) 0.2 mM. All the chromatograms were performed in isocratic mode. The MagicPlot Student software was used for the resolution of “problem” (with a low value of RS) TAG.
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