Geumgang pine (Pinus densiflora Sieb. At Zucc., red pine) from the lower branches of a single 15∼18 year old tree was harvested in the mountains at an elevation of 580 m, Uljin, Gyeongbuk, Korea. The successive harvestings occurred in May (spring), August (summer), October (autumn), and January (winter) in 2020. Haesong pine (Pinus thunbergii Parlatore, black pine) was also harvested in the seashore of Sokcho, Uljin, and Yeongduk, Korea. Two pine trees were identified by President in Southern Regional Office of Forest Service, National Institute Forest Science (Uljin, Korea), and a voucher specimen was deposited at the Department of Food Science and Nutrition, Catholic University. The needles were separated from the branches and instantly freeze-dried. Nuclear magnetic resonance (NMR) solvents were obtained from Sigma Chemical Co. (St. Louis, MO, USA). All solvents for HPLC analysis were of Merck HPLC grade (Merck, Kenilworth, NJ, USA). All other reagents used in this study were of analytical grade.
Nmr solvents
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NMR solvents are a class of chemical compounds used in nuclear magnetic resonance (NMR) spectroscopy. They serve as the media in which the sample to be analyzed is dissolved, enabling the acquisition of NMR data. NMR solvents are selected based on their compatibility with the specific sample and their ability to maintain the chemical and physical properties of the analyte during the NMR analysis.
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Lab products found in correlation
6 protocols using nmr solvents
1
Seasonal Variation of Geumgang and Haesong Pine Needles
2
Gallium-Bound Mycobactin-Like Siderophore Characterization
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NMR solvents were obtained from Sigma-Aldrich and used without further purification.
For NMR analysis, 1.5 mg gallium sulfate was dissolved in 3 ml deuterated methanol and then incubated with the mycobactin-like siderophore overnight. The solvent was removed in vacuo, and the Ga-bound species was resuspended in CDCl3 for NMR analyses. Chemical shift signals (δ) are reported in parts per million and are referenced to the internal chloroform signal (δ = 7.26 ppm for 1H; δ = 77.2 ppm for 13C).
For NMR analysis, 1.5 mg gallium sulfate was dissolved in 3 ml deuterated methanol and then incubated with the mycobactin-like siderophore overnight. The solvent was removed in vacuo, and the Ga-bound species was resuspended in CDCl3 for NMR analyses. Chemical shift signals (δ) are reported in parts per million and are referenced to the internal chloroform signal (δ = 7.26 ppm for 1H; δ = 77.2 ppm for 13C).
3
Synthetic Characterization and Biological Assays
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All reagents
used for chemical synthesis were purchased from commercially
available sources and used without further purification. Nuclear magnetic
resonance (NMR) solvents were obtained from Sigma-Aldrich. 1H, 13C, and 19F NMR spectra were recorded on
a Varian MERCURY 400 spectrometer (400 MHz for 1H NMR,
101 MHz for 13C NMR, and 376 MHz for 19F NMR).
Chemical shifts (δ) are expressed in parts per million (ppm)
downfield from tetramethylsilane, and deuterated solvent signal was
used as reference. Coupling constants (J) are expressed
in hertz (Hz). Abbreviations used are s = singlet, bs = broad singlet,
d = doublet, dd = doublets of doublets, t = triplet, td = triplets
of doublets, q = quartet, and m = multiplet. Mass spectra were obtained
at the “Centres Científics i Tecnològics de la
Universitat de Barcelona” (CCiTUB). Compounds tested in the
different biological assays were previously diluted to a stock concentration
of 0.5 to 1 M in H2O to perform the experiments.
used for chemical synthesis were purchased from commercially
available sources and used without further purification. Nuclear magnetic
resonance (NMR) solvents were obtained from Sigma-Aldrich. 1H, 13C, and 19F NMR spectra were recorded on
a Varian MERCURY 400 spectrometer (400 MHz for 1H NMR,
101 MHz for 13C NMR, and 376 MHz for 19F NMR).
Chemical shifts (δ) are expressed in parts per million (ppm)
downfield from tetramethylsilane, and deuterated solvent signal was
used as reference. Coupling constants (J) are expressed
in hertz (Hz). Abbreviations used are s = singlet, bs = broad singlet,
d = doublet, dd = doublets of doublets, t = triplet, td = triplets
of doublets, q = quartet, and m = multiplet. Mass spectra were obtained
at the “Centres Científics i Tecnològics de la
Universitat de Barcelona” (CCiTUB). Compounds tested in the
different biological assays were previously diluted to a stock concentration
of 0.5 to 1 M in H2O to perform the experiments.
4
Seasonal Variations in Red and Black Pine Chemistry
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Geumgang pine (P. densiflora Sieb. At Zucc., red pine) from the lower branches of a single 15- to 18-year-old tree was harvested in the mountains in May (spring) and October (autumn) in 2020 at an altitude of 580 m, Uljin, Gyeongbuk, Korea. In addition, two other red pines in Yeongdeok and Cheongsong regions are also collected during two seasons compared to black pine. Additionally, Haesong pine (P. thunbergii Parlatore, black pine) was also harvested in May and October along the seashore of Sokcho, Samchuk, Uljin, Yeongdeok, and Pohang, Korea. In the Southern Regional Office of the Forest Service, National Institute of Forest Science (Uljin, Korea), two pine trees were identified by the president, and an authenticated voucher specimen was kept in the Department of Food Science and Nutrition, Daegu Catholic University. The twigs below 1-cm diameter were separated from two pine trees after removing pine needles and cut into small pieces by a mechanical cutter. The cut twigs were dried in the shade for 1 week and then finally dried in the dry oven at 45±5°C. Nuclear magnetic resonance (NMR) solvents were obtained from Sigma Chemical Co. (St. Louis, MO, USA). All solvents for HPLC analysis were of Merck HPLC grade (Merck, Kenilworth, NJ, USA). All other reagents used in this study were of analytical grade.
5
Synthesis of Fluorinated Phenylalanine Derivatives
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All chemicals and solvents are commercially available and were used as supplied unless otherwise stated. All amino acids (L-phenylalanine, L & D-4 fluoro phenylalanine) were purchased from Chem Impex, Inc. (Wood Dale, IL, USA). 1-Hydroxybenzotriazole (HOBt) and dicyclohexylcarbodiimide (DCC) were purchased from Alfa-Aesar (Ward Hill, MA, USA). All NMR solvents were purchased from Sigma-Aldrich (St. Louis, MO, USA).
6
Purification and Characterization Techniques
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Solvents used for the purification procedure, gradient solvents used for HPLC analyses and NMR solvents were purchased from Sigma-Aldrich. Evaporation was carried out under vacuum using a rotating evaporator. Silica gel flash chromatography was performed using silica gel 60 Å (0.040-0.063 mm; MERK). Thin layer chromatography (TLC) analysis was carried on Merck aluminium silica gel (60 F254) TLC plates that were visualized under a UV lamp (λ = 254 nm) or by spraying with a 10 % solution of phosphomolybdic acid in absolute ethanol. Preparative thin layer chromatography (Prep TLC) purification was performed using either 2 mm (20 x 10) and 1 mm (10 x 10) glass-backed sheets pre-coated with silica gel 60 F254 purchased from VWR.
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