All reagents and solvents were purchased from either Sigma-Aldrich (Milwaukee, WI) or Fisher Scientific (Pittsburgh, PA). 1H NMR spectra were recorded on a Bruker Ultrashield 400 or 500 MHz spectrometer. ESI mass spectra were obtained on a Bruker Esquire 3000 plus system. High-resolution mass spectrometry (HR-MS) was done by the Mass Spectrometry Facility at the University of Notre Dame using ESI by direct infusion on a Bruker micrOTOF-II. High performance liquid chromatography (HPLC) purification was performed on a Varian Prostar System. [18F]Fluoride was produced by 18 MeV proton bombardment of a high pressure [18O]H2O target using a General Electric PET trace biomedical cyclotron (Milwaukee, WI). [18F]DCFPyL was prepared as previously published.14 (link) Reverse phase radio-HPLC purification was performed using a Varian Prostar System with a Bioscan Flow Count PMT radioactivity detector (Varian Medical Systems, Washington, DC). Radioactivity was measured in a Capintec CRC-10R dose calibrator (Ramsey, NJ). The specific radioactivity was calculated as the radioactivity eluting at the retention time of the product during the semipreparative HPLC purification divided by the mass (determined from a standard curve) corresponding to the area under the curve of the UV absorption.
Prostar system
Manufactured by Agilent Technologies
Sourced in United States, Netherlands, Australia, United Kingdom
The ProStar system is a suite of analytical instruments designed for laboratory applications. It provides precise and reliable measurements to support various scientific and industrial workflows. The core function of the ProStar system is to enable accurate data collection and analysis for researchers and technicians working in diverse fields.
Automatically generated - may contain errors
Lab products found in correlation
Esquire 3000 plus system, by Bruker (2 mentions)
Ultrashield 400, by Bruker (1 mentions)
Microtof 2, by Bruker (1 mentions)
Whatman no 4, by Cytiva (1 mentions)
Whatman, by Cytiva (1 mentions)
Galaxie workstation software, by Agilent Technologies (1 mentions)
Avance 500 mhz spectrometer, by Bruker (1 mentions)
Vnmrs spectrometer, by Agilent Technologies (1 mentions)
Ft ir 4100 spectrometer, by Jasco (1 mentions)
Avance 600 mhz, by Bruker (1 mentions)
Irdye 700dx nhs ester, by LI COR (1 mentions)
Snakeskin dialysis tubing, by Thermo Fisher Scientific (1 mentions)
Openlab cds software, by Agilent Technologies (1 mentions)
C4 column, by Phenomenex (1 mentions)
Ni nta agarose, by Qiagen (1 mentions)
Enterokinase, by New England Biolabs (1 mentions)
Advancebio oligonucleotide column, by Agilent Technologies (1 mentions)
Agilent 6530 accurate mass q tof lc ms, by Agilent Technologies (1 mentions)
Metronidazole, by Merck Group (1 mentions)
Openlab cds chemstation software, by Agilent Technologies (1 mentions)
17 protocols using prostar system
1
Radiolabeling and Purification of [18F]DCFPyL
2
Fumonisins Quantification in Samples
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Fumonisins were measured by using the method for the extraction of AOAC Official Method 995.15 and the quantification by LC-FLD is described in [67 (link)] in ISPA-CNR. For each sample, 12.5 g of our sample were extracted with 50 mL methanol/water (75/25, v/v) by shaking for 60 min at 250 rpm. The extract was filtrated through filter paper (Whatman no. 4, Maidstone, VT, USA) and the pH of the extract was measured and adjusted to 5.8–6.5. Ten milliliters of filtrate were applied to strong anion-exchange (500 mg SAX, Varian Inc., Palo Alto, CA, USA) cartridge previously conditioned by successive washing with 5 mL methanol and 5 mL methanol/water (75/25, v/v) followed by 8 mL of methanol/water (75/25, v/v) and 3 mL of methanol. Fumonisins were eluted with 10 mL of 1% acetic acid in methanol. The elutes were evaporated to dryness under a stream of nitrogen at 50 °C. The residues were dissolved with 500 µL of acetronirile/water (30/70, v/v). The HPLC apparatus consisted of a ProStar system (Varian Inc., Palo Alto, CA, USA) equipped with a fluorometric detector set at wavelengths, ex = 335 nm, em = 440 nm. The column was a SymmetryShield C18 (150 mm × 4.6 mm, 5 µm particle size) with a guard column inlet filter (0.5 µm × 3 mm diameter, Rheodyne Inc., Rohnert Park, CA, USA). Detection limit for fumonisins was 2 µg/kg.
3
Oligonucleotide Purification and Analysis
4
Radiolabeling of Peptide Tracer WL12 with Cu-64
5
Peptide Purification by Reverse Phase HPLC
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The peptides were analyzed and purified
via reverse phase HPLC using either a Varian ProStar system with a
model 210 solvent delivery module and a model 320 UV detector or a
Dionex system with a PDA-100 photodiode array detector and a model
ASI-100 automated sample injector. The preparative purification was
performed using an ACE C8-300 semipreparative column (150 × 10
mm, flow rate of 8.0 mL/min), with UV detection at 215 and 254 nm,
loaded with 200–1850 μL aliquots of a 10–20 mg/mL
solution of peptide dissolved in water. Gradient conditions are reported
for each peptide. The fractions containing the correct peak were pooled,
the solvent was removed under reduced pressure to approximately 2
mL, and the solution was freeze-dried.
via reverse phase HPLC using either a Varian ProStar system with a
model 210 solvent delivery module and a model 320 UV detector or a
Dionex system with a PDA-100 photodiode array detector and a model
ASI-100 automated sample injector. The preparative purification was
performed using an ACE C8-300 semipreparative column (150 × 10
mm, flow rate of 8.0 mL/min), with UV detection at 215 and 254 nm,
loaded with 200–1850 μL aliquots of a 10–20 mg/mL
solution of peptide dissolved in water. Gradient conditions are reported
for each peptide. The fractions containing the correct peak were pooled,
the solvent was removed under reduced pressure to approximately 2
mL, and the solution was freeze-dried.
6
HPLC Analysis of Histamine in Cheese
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The content of histamine was analysed by high performance liquid chromatography using the Pro Star system (Varian, Netherlands) equipped with a diode array detector, quaternary pump, autosampler, and column thermostat, and controlled by the Galaxie Workstation software (Varian). The chromatographic separation was performed on a Unisol C18 column of 150 × 4.6 mm, particle size 3 μm, connected to a C18 precolumn of 10 × 3 mm (Agela Technologies, USA). The mobile phase, consisting of 15% methanol in 0.1 M potassium dihydrogen phosphate (150/850, v/v) with 1.6 mM 1-octanesulphonic acid, was applied under isocratic conditions. The column oven temperature was maintained at 25°C, the flow rate at 0.5 mL/min, and the injection volume was 20 μL. The UV detection was monitored at 215 nm.
The range of the method for hard cheeses was 4.25–420 mg/kg and the limits of detection and quantification were 3.52 mg/kg and 4.25 mg/kg respectively, whereas the range of the method for mould cheeses was 7.13–420 mg/kg and the limits of detection and quantification were 6.27 mg/kg and 7.13 mg/kg respectively. The repeatability (n = 6) and the reproducibility (n = 18) for hard cheeses were 3.6% and 4.6% respectively, whereas for mould cheeses these parameters were 1.9% and 3.0%. Recovery of the method ranged from 80.1% for hard cheeses to 82% for mould cheeses.
The range of the method for hard cheeses was 4.25–420 mg/kg and the limits of detection and quantification were 3.52 mg/kg and 4.25 mg/kg respectively, whereas the range of the method for mould cheeses was 7.13–420 mg/kg and the limits of detection and quantification were 6.27 mg/kg and 7.13 mg/kg respectively. The repeatability (n = 6) and the reproducibility (n = 18) for hard cheeses were 3.6% and 4.6% respectively, whereas for mould cheeses these parameters were 1.9% and 3.0%. Recovery of the method ranged from 80.1% for hard cheeses to 82% for mould cheeses.
7
Analytical Characterization of Chemical Compounds
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All chemicals were purchased from Sigma–Aldrich or Alfa Aesar and were used without further purification. Thin Layer Chromatography (TLC): precoated aluminium backed plates (60 F254, 0.2 mm thickness, Merck) were visualized under both short and long wave UV light (254 and 366 nm). Flash column chromatography was carried out using silica gel supplied by Fisher (60A, 35–70 μm). Analytical High Performance Liquid Chromatography (HPLC) analysis was performed using either a ThermoScientific or a Varian Prostar system. 1H NMR (500 MHz), 13C NMR (125 MHz) and 19F NMR (470 MHz) spectra were recorded on a Bruker Avance 500 MHz spectrometer at 25 °C. Chemical shifts (δ) are expressed in parts per million (ppm) and coupling constants (J) are given in hertz. The following abbreviations are used in the assignment of NMR signals: s (singlet), bs (broad singlet), d (doublet), t (triplet), q (quartet), qn (quintet), m (multiplet), dd (doublet of doublet), dt (doublet of triplet), td (triple doublet), dq (double quartet), m (multiplet), dm (double multiplet). Mass spectrometry was run on a Bruker Micromass system in electrospray ionisation mode. Accurate mass spectrometry was performed at the EPSRC UK National Mass Spectrometry facility at Swansea University. Elemental analysis (% C, H, N) was run at Medac Ltd. (Chobham, Surrey, U.K.) as an external service.
8
Spectroscopic Characterization of Organic Compounds
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UV spectra were obtained in MeOH using a Varian Cary 50 spectrometer and IR spectra on a JASCO FT/IR 4100 spectrometer. All NMR spectra were recorded on a Varian VNMRS spectrometer (500 and 125 MHz for 1H and 13C NMR, respectively) in CDCl3. Proton and carbon chemical shifts were referenced versus 7.26 and 77.0 ppm, respectively. Electrospray ionization mass spectroscopy/mass spectroscopy (ESIMS/MS) spectra were acquired in enhanced product ion mode using an AB SCIEX QTRAP 3200 unit at an ion source potential of 5500 V, a declustering potential of 60 V, and a collision energy of 35 eV. HPLC was performed using a Varian Prostar system equipped with a 355 refractive index detector and either a YMC-pack ODS-H80 (5 μm, 150 × 4.6 mm) or a YMC-pack Si (5 μm, 250 × 10.0 mm) column.
9
HPLC Analysis and Purification Protocol
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All chemical reagents and solvents were taken from commercial sources and used without purification. High-performance liquid chromatography analyses were carried out on a Waters Binary Module System (Waters, Milford, MA, USA) with a dual λ absorbance detector system fitted with a Supelco Ascentis C8 HPLC column (250 mm × 4.6 mm, 5 µm, Supelco, Bellefonte, PA, USA) with a 1 mL/min flow rate operating on a linear gradient from 5 to 95% B within 20 min (solvent A: H2O with 0.05% trifluoroacetic acid, solvent B: MeCN with 0.05% trifluoroacetic acid). High-performance liquid chromatography purification was carried out in a Varian ProStar system (Varian, Australia) with a dual λ absorbance detector system with the application of a Supelco Ascentis C8 HPLC column (250 mm × 21.2 mm, 5 µm) with a 15 mL/min flow rate and a linear gradient from 20 to 100% B within 20 min or 40 to 100% B within 20 min (depending on compound solubility), solvent A: H2O with 0.05% trifluoroacetic acid, solvent B: MeCN with 0.05% trifluoroacetic acid. The nuclear magnetic resonance spectra (1H and 31P) were recorded on a 400 MHz NMR Jeol PCZ 400S or Bruker Avance 600 MHz (Bruker, Billerica, MA, USA). High resolution mass spectra were recorded with a Brucker micro TOF-Q II (Bruker, Billerica, MA, USA).
10
Synthesis and Characterization of Fluorescent Probe
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