Actus triart c18 column

ADS790WS is 2-[2-[2-(4-aminobenzenethio)-3-[(1,3-dihydro-3,3-dimethyl-1-(4-sulfobutyl)-2H-indol-2-ylidene)-ethylidene]-1-cycloxen-1-yl]-ethynyl]-3,3-dimethyl-1-(4-sulfobutyl)-3H-indolium, innersalt, monosodium, which was purchased from American Dye Source, Inc. (Montreal, QC, Canada). DOTA-NHS-ester (1,4,7,10-Tetraazacyclododecane- 1,4,7,10-tetraacetic acid mono-N-hydroxysuccinimide ester) was purchased from Macrocyclics (Dallas, TX, USA). The ESI (electrospray ionization) mass spectral data were collected on a AB Sciex 4000QTrap system (Concord, ON, Canada). ¹¹¹InCl₃ (indium chloride in 0.05 M HCl) was purchased from Institute of Nuclear Energy Research (INER), Taoyuan, Taiwan. ¹⁷⁷LuCl₃ was purchased from perkin elmer (Waltham, MA, USA).
Preparative reversed-phase high performance liquid chromatography (HPLC) was performed on a SHIMADZU Prominence Preparative HPLC System with a SHIMADZU SPD-20AV detector using YMC-Actus Triart C18 column (5 μm, 250 × 20 mm). Analytic reversed-phase HPLC was performed on a Waters 2695 Separations Module with a Waters 2487 Dual Wavelength Absorbance Detector plus a Bioscan radioisotope detector using YMC-Triart C18 column (5 μm, 250 × 4.6 mm). Waters Bridge column (5 μm, 200 ×4.6 mm). The flow rate was 20 mL/min for the preparative column and 1 mL/min for the analytic column running wth 60% ACN and 40% water with 0.1% TFA.

EC, ECG, EGC, EGCG, TF, TF3G, TF3′G, and TFDG were purchased from FUJIFILM Wako Pure Chemical Corporation (Osaka, Japan). TSA was synthesized from EGCG and purified as described [26 (link)]. Briefly, a solution of EGCG (1.0 g, 2.18 mmol) and CuCl₂ (269 mg, 2.00 mmol) in 30% MeOH (400 mL) was vigorously mixed for 24 h. To the reaction mixture, ascorbic acid (10 g) was added and heated at 85 °C for 15 min. After chilling, the mixture was concentrated to evaporate MeOH and the resulting aqueous solution was applied to a Diaion HP20 column (Mitsubishi Chemical Corp., Tokyo, Japan, 3.0 cm i.d. × 25 cm) with water. After washing the column with water to remove reagents, sample was eluted with 70% MeOH (300 mL), and applied to a preparative high-performance liquid chromatography (HPLC) using a YMC-Actus Triart C18 column (YMC Co., Ltd., Kyoto, Japan, 20 mm i.d. × 250 mm). To elute the column, isocratic elution method was performed using a solvent mixture of water: CH₃CN = 3:2 at a flow rate of 16 mL/min. LC chromatograms were obtained at UV 280 nm. The fraction of TSA was collected and freeze-dried. The yield and purity of TSA were 251 mg and 96%, respectively.

Deionized water was used for all experiments. Proton nuclear magnetic resonance (¹H NMR) experiments were performed on a Bruker Advance 500 spectrometer. Chemical shifts were given as d values with reference to tetramethylsilane (TMS) as an internal standard. Coupling constants were given in Hz. High-resolution fast atom bombardment mass (FAB mass) spectra were obtained from the Korean Basic Science Institute using a JMS-700 model (Jeol, Japan) mass spectrometer. A preparative high-pressure liquid chromatography (prep-HPLC; LC/Forte/R, YMC, Japan) system equipped with a YMC-Actus Triart C₁₈ column (250 × 20.0 mm. inner diameter, S-5 µm, 12 nm, YMC, Japan) was used for purification. The prep-HPLC system used ultraviolet–visible (UV–vis) detection at 330 and 365 nm. The purity of all products was determined to be above 95% by the HPLC spectra. A flash column chromatography system (Isolera Prime, Biotage, Uppsala, Sweden) with SNAP KP-C₁₈-HS 12 g was used for purification. The system used UV–vis detection at 254 and 330 nm. Gd concentration data used to confirm lipophilicity were measured using the Optima 7300DV and Avio 500 inductively coupled plasma (ICP) spectrometers (Perkin Elmer, Waltham, MA, USA). UV–vis absorption and fluorescence measurements were performed with a SpectraMax^® i3 (Molecular Devices, San Jose, CA, USA) using 96-well cell culture plates at 25 °C.