A sample solution of rotenone (1.0 g) in H2O (2.0 L) in capped vials was autoclaved at 121°C for 12 h. The dried reactant was directly subjected to column chromatography over a YMC GEL ODS AQ 120-50S column (1.1 cm i.d. × 36 cm) with aqueous MeOH to yield pure (-)-tubaic aid (16.6 mg). High-performance liquid chromatography (HPLC) analysis was performed on a YMC-Pack ODS A-302 column (4.6 mm i.d. × 150 mm; YMC Co., Ltd.), which consisted of a linear gradient that started with 10% (v/v) MeCN in 0.1% HCOOH/H2O (detection: UV 280 nm; flow rate: 1.0 ml/min; at 40°C), increased to 80% MeCN over 23 min, and then to 100% MeCN over 5 min. The structure of the newly generated compound was determined based on the interpretation of the spectroscopic data.
Pack ods a 302 column
Manufactured by YMC
Sourced in United States
The YMC-Pack ODS A-302 column is a reversed-phase liquid chromatography column designed for the separation and analysis of a wide range of chemical compounds. The column features a silica gel stationary phase with covalently bound octadecyl (C18) ligands, providing a stable and efficient platform for reversed-phase separations.
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Lab products found in correlation
Gel ods aq 120 50s, by YMC (2 mentions)
Gel ods aq 120 50s column, by YMC (1 mentions)
High performance liquid chromatography (hplc), by Shimadzu (1 mentions)
U 2000 spectrophotometer, by Hitachi (1 mentions)
Phloroglucinol, by Merck Group (1 mentions)
Vns600 instrument, by Agilent Technologies (1 mentions)
5 protocols using pack ods a 302 column
1
Preparation and Purification of (-)-Tubaic Acid
2
HPLC-PDA Analysis of Herbal Compounds
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High-performance liquid chromatography (HPLC) (Shimadzu, Tokyo, Japan) combined with a photodiode array (PDA) detector was used for the chromatographic analysis of HRT. The HPLC analysis was performed using a YMC-Pack ODS A-302 column (4.6 mm i.d. × 150 mm; YMC, Co., Kyoto, Japan), and the solvent system consisted of a gradient mode with an initial 10% CH3CN with 10 mM phosphate buffer increased to CH3CN over 120 min (temperature: 40°C; flow rate: 1.0 mL/min; UV detection; 280 nm). Successive column chromatography was conducted using YMC GEL ODS AQ 120-50S (YMC, Co., Kyoto, Japan). Quantification of the five standard compounds was carried out by HPLC analysis using the external standard method by constructing standard curves. Five concentrations were used for preparation of the calibration curve and the calibration curve of pure solutions of the selected compounds was completely linear (R2 > 0.999). Five concentrations were used for preparation of the calibration curve and the calibration curve of pure solutions of the all standard compounds was completely linear (R2 > 0.999). The retention times of geniposide (1 ) (tR 5.3 min), coptisine (2 ) (tR 17.9 min), palmatine (3 ) (tR 35.5 min), berberine (4 ) (tR 32.2 min), and baicalin (5 ) (tR 45.1 min) were then detected at 240 and 277 nm.
3
Preparation and Purification of Rotenoisin A
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Rotenoisin A was prepared using the method described in our previous report [15 (link)]. Briefly, a sample solution of rotenone (0.5 g) in MeOH (200 ml) in capped vials was exposed to 50 kGy (absorbed dose) of radiation. Irradiation was carried out at ambient temperature using a cobalt-60 irradiator (point source AECL, IR-79, MDS Nordion International Co. Ltd, Ottawa, ON, Canada) at the Advanced Radiation Technology Institute, Korea Atomic Energy Research Institute (Jeongup, Korea). The source strength was ~320 kCi, with a dose rate of 10 kGy h–1 at the location of the sample. The irradiated methanolic solution was immediately evaporated to remove the solvent and lyophilized. The dried irradiated solution was directly subjected to column chromatography over a silica gel column (2.5 cm i.d. × 32 cm) with CHCl3-MeOH–MeOH to yield pure rotenoisin A (129.1 mg, retention time 4.5 min). HPLC analysis was carried out on a YMC-Pack ODS A-302 column (4.6 mm i.d. × 150 mm; YMC Co., Ltd) and was developed at 40°C with 1% HCOOH/MeCN (1:1, flow rate 1.0 min–1, detection 280 nm).
4
Radiation-Induced Dexamethasone Degradation
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One gram of stock solution of Dex dissolved in 1 L of methanol was irradiated by ionizing radiation with γ-rays in a 60Co γ-chamber for 2 h for a total dose of 20 kGy with a dose rate of 10 kGy h-1. The samples were irradiated at room temperature (RT) in air using a 60Co irradiator (MDS Nordion, Ottawa, ON, Canada). After evaporation in vacuo, the samples were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) or high-performance liquid chromatography (HPLC) to determine the novel fraction of γ-irradiated Dex components by comparing the chromatogram with that of the original Dex. The LC-MS/MS (Agilent Technologies, Palo Alto, CA, USA) analysis was performed in a YMC-Pack ODS A-302 column (4.6 mm i.d. × 150 mm; YMC, Kyoto, Japan) and the solvent system consisted of a linear gradient that started with 0.1% HCOOH (detection: UV 254 nm; flow rate: 1.0 mL/min; at 40°C), was increased to 50% (v/v) MeCN in 0.1% HCOOH/H2O over 20 min, and then increased to 100% MeCN over 20 min [13 (link)]. At the end of a run, an additional 15 min was used to allow equilibration of the column. This γ-irradiated Dex was named Dex-IR and five main peaks were detected.
5
Spectroscopic Analysis of (-)-EGCG and Phloroglucinol
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General Experimental Procedures (-)-EGCG and phloroglucinol were obtained from Sigma-Aldrich (St. Louis, MO, U.S.A.). UV spectra were run on a Hitachi U-2000 spectrophotometer (Hitachi, Tokyo, Japan) and CD spectra were recorded on a JASCO J-720W spectrometer (JASCO Inc., Tokyo, Japan). NMR spectroscopic data were recorded at room temperature on a Varian VNS600 instrument (Varian, Palo Alto, CA, U.S.A.). Chemical shifts are provided in δ (ppm) values relative to those of the solvent acetone-d 6 (δ H 2.04; δ C 29.8) on a tetramethylsilane scale. The standard pulse sequences programmed into the instruments were used for each 2D measurement. The J CH value was fixed at 7 Hz in the HMBC spectra. FABMS were performed on a Micro Mass Auto Spec OA-TOF mass spectrometer (Micromass, Manchester, U.K.) operated in the negative-ion mode. Column chromatography was conducted using YMC GEL ODS AQ 120-50S (YMC Co., Kyoto, Japan). Reversed-phase HPLC analysis was operated on a YMC-Pack ODS A-302 column (4.6 mm i.d. × 150 mm; YMC Co.).
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