Both THF and diethyl ether were freshly distilled from sodium and benzophenone, while acetonitrile, methylene chloride, pyridine, and triethylamine (Et3N) were distilled from calcium hydride prior to use. Toluene and DMF were dried over molecular sieves prior to use. All other reagents and solvents were purchased from commercial sources and used without further purification. All reactions were conducted in flame or oven dried glassware under a positive pressure of argon and with magnetic stirring. The NMR spectra were obtained at 400 MHz for 1H, 75, 100, or 125 MHz for 13C, and 121 or 161 MHz for 31P. Internal standards of Si(CH3)4 (1H, 0.00 ppm) or CDCl3 (1H, 7.27 ppm; 13C, 77.2 ppm) were used. The 31P chemical shifts are reported in ppm relative to 85% H3PO4 (external standard). High resolution mass spectra were obtained at the University of Iowa Mass Spectrometry Facility. Silica gel (60 Å, 0.040–0.063 mm) was used for flash chromatography. The HPLC separations were carried out using a Beckman System Gold instrument with a model 166 variable wavelength UV detector connected to a 128 solvent module.
System gold instrument
Manufactured by Beckman Coulter
Sourced in United States
The System Gold instrument is a high-performance liquid chromatography (HPLC) system designed for analytical and preparative applications. It provides precise control and monitoring of the chromatographic separation process, enabling accurate and reproducible results.
Automatically generated - may contain errors
Lab products found in correlation
4 protocols using system gold instrument
1
Purification and Characterization of Organic Compounds
2
Synthesis of DOX-5FU Conjugate
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DOX*HCl (38 mg, 0.065 mmol) and TFA (3 µl, 0.04 mmol) were added to 1-carboxymethyl-5-fluorouracil hydrazide (40 mg, 0.13 mmol) in 12 ml of absolute methanol at stirring. The reaction mixture was stirred in the darkness for 24 h at room temperature, then it was concentrated in vacuo to 3 ml, and 9 ml of acetonitrile was added. After cooling for 12 h at 0°C, the obtained precipitate was filtered and purified by phase reverse HPLC using System Gold instrument (Beckman, USA) and YMC-Triart C18 column (5 µm, 250 x 10 mm). The mobile phase consisted of acetonitrile/water (85:15 v/v). Flow rate was fixed at 1 ml/min for analytical and 10 ml/min for preparative chromatography. Detection was performed by UV spectroscopy at 220 nm. The fractions containing the final product were combined and evaporated under the reduced pressure. The yield of DOX-5FU was 14 mg (15%).
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DOX*HCl (38 mg, 0.065 mmol) and TFA (3 µl, 0.04 mmol) were added to 1-carboxymethyl-5-fluorouracil hydrazide (40 mg, 0.13 mmol) in 12 ml of absolute methanol at stirring. The reaction mixture was stirred in the darkness for 24 h at room temperature, then it was concentrated in vacuo to 3 ml, and 9 ml of acetonitrile was added. After cooling for 12 h at 0°C, the obtained precipitate was filtered and purified by phase reverse HPLC using System Gold instrument (Beckman, USA) and YMC-Triart C18 column (5 µm, 250 x 10 mm). The mobile phase consisted of acetonitrile/water (85:15 v/v). Flow rate was fixed at 1 ml/min for analytical and 10 ml/min for preparative chromatography. Detection was performed by UV spectroscopy at 220 nm. The fractions containing the final product were combined and evaporated under the reduced pressure. The yield of DOX-5FU was 14 mg (15%).
3
Tc-99m Compound RCP Analysis by HPLC
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The RCP of the final Tc-99m compounds was determined by HPLC performed on a Beckman System Gold Instrument equipped with a programmable solvent Module 126, scanning detector Module 166, and a radioisotope detector Module 170. Chromatographic analyses were carried out on a reversed-phase Agilent precolumn Zorbax 300SB-C18 (4.6 × 12.5 mm) and a reversed-phase Agilent column Zorbax 300SB-C18 (4.6 × 250 mm) using the following conditions. Mobile phase: A = water containing 0.1% TFA, B = acetonitrile containing 0.1% TFA; gradient: 0 min, B = 0%; 0–25 min, B = 100%; 25–30 min, B = 100%; 30–35 min, B = 0%; flow rate: 1.0 mL/min.
4
Liposomal Encapsulation of D6-Chol
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D6-Chol was entrapped into oligolamellar, 280-300 nm-wide liposomes, following the dehydrationrehydration method [22, (link)23] (link). Briefly, D6-Chol and PC were dissolved in chloroform at 1:1 molar ratio. After solvent evaporation, the lipid film was rehydrated and ultracentrifuged at 100,000 g for 35 min at 4°C to separate residual lipids. Liposomes were resuspended with 10 mM phosphate buffered saline, pH 7.4. The concentration of D6-Chol entrapped in liposomes was determined by HPLC (System Gold instrument -Beckman) equipped with an Eco Cart-LiChrospher® 60 RP-select B column (125 × 3 mm, particle size 5 µm, pore size 60 Å, Merck) at 214 nm. Separation was done with isocratic elution at 100% methanol:isopropanol:NH4OH (70%:30%, 5mM) for 12 min. The flow rate was 0.6 mL/min. Entrapment efficacy was ±90%, and liposomes were diluted to a final D6-Chol concentration of 5.6 mg/mL.
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