Optical rotations were obtained on a JASCO-2000 Polarimeter (Hachioji, Japan). UV spectra were recorded on a Shimadzu UV-1800 spectrophotometer (Shimadzu, Kyoto, Japan). The NMR spectra were recorded on a Bruker Avance Neo 600 spectrometer operating at 600 MHz for 1H and 150 MHz for 13C. The HRESIMS data were recorded on SCIEX X500 QTOF (SCIEX, MA, USA) mass spectrometer. Silica gel (60 N, spherical, neutral, 40–50 mm, Kanto Chemical Co., Inc., Tokyo, Japan), YMC RP-18 (Fuji Silysia Chemical Ltd, Kasugai, Aichi, Japan), Sephadex LH-20 (DowexVR 50WX2-100, Sigma-Aldrich, USA) were used to remove the pigment and for coarse separation. Precoated silica gel plates (Merck, Kieselgel 60 F254, 0.25 mm) and precoated RP-18 F254s plates (Merck) were used for analytical thin-layer chromatography analyses. Five human cancer cell lines, including breast carcinoma (MCF-7), hepatocellular carcinoma (HepG2), lung carcinoma (LU-1), gastric adenocarcinoma (AGS), colon adenocarcinoma (SW-480), and human embryonic kidney cells (HEK-293A) were obtained from the American Type Culture Collection (ATCC, Manassas, VA, USA).
Precoated rp 18 f254s plates
Manufactured by Merck Group
Sourced in Germany
Precoated RP-18 F254s plates are a type of thin-layer chromatography (TLC) plates used for analytical and preparative separation of compounds. The plates are pre-coated with a reversed-phase (RP-18) stationary phase and contain a fluorescent indicator (F254s) that allows for UV detection of separated compounds.
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Lab products found in correlation
Unity plus 500 spectrometer, by Agilent Technologies (2 mentions)
Jms700n, by JEOL (2 mentions)
Jms 100td, by JEOL (2 mentions)
Mcf 7, by American Type Culture Collection (1 mentions)
Sw480, by American Type Culture Collection (1 mentions)
Uv 1800 spectrophotometer, by Shimadzu (1 mentions)
Hek293a, by American Type Culture Collection (1 mentions)
Mci gel chp 20p, by Merck Group (1 mentions)
Lichroprep rp 18, by Merck Group (1 mentions)
Jms 700 instrument, by JEOL (1 mentions)
P 2300 polarimeter, by Jasco (1 mentions)
C18 column, by Merck Group (1 mentions)
Acd nmr processor academic edition software, by Advanced Chemistry Development (1 mentions)
5 protocols using precoated rp 18 f254s plates
1
Spectroscopic Analysis of Anticancer Compounds
2
NMR Characterization of Organic Compounds
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The NMR spectra were obtained at 400 and 100 MHz for 1H and 13C, respectively, on a Varian MR 400 NMR spectrometer (Agilent Technologies, Santa Clara, CA, USA) in CDCl3 or pyridine-d5, with solvent peaks as references. Silica gel 60 (Merck Millipore, 230–400 mesh), MCI gel CHP20P (Merck Millipore, 75–150 μm), and LiChroprep RP-18 (Merck Millipore, 40–63 μm) were used for column chromatography. Precoated silica gel plates (Merck Millipore, Kieselgel 60 F254, 0.25 mm) and precoated RP-18 F254s plates (Merck Millipore, 1.05560) were employed in TLC analyses. Spots were visualized under ultraviolet (UV) light or heating silica gel plates sprayed with 10% H2SO4 in CH3OH. High-performance liquid chromatography (HPLC) was performed on a Primaide 1110 pump equipped with a Primaide 1410 UV detector at 220 nm and a semipreparative reversed-phase column (Merck Millipore, Hibar Purospher RP-18e, 5 μm, 250 mm × 10 mm).
3
Structural Analysis of Natural Compounds
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Sephadex LH-20 (Pharmacia Fine Chemical Co. Ltd) was used for column chromatography. Precoated silica gel plates (Merck, Kieselgel 60 F254, 0.25 mm) and precoated RP-18 F254s plates (Merck) were used for thin-layer chromatography (TLC) analysis. High resolution FAB-MS and ESI-MS were recorded on JEOL JMS700N and JMS-100TD, respectively. 1H- and 13C-NMR, 1H-1H COSY, NOESY, HSQC, and HMBC spectra were recorded with a Unity plus 500 spectrometer (Varian Inc., U.S.A.) operating at 500 MHz for 1H and 125 MHz for 13C, respectively. 1H-NMR chemicals shifts are expressed in δ values referring to the solvent peak δH 2.49 for DMSO and coupling constants are expressed in Hz. 13C-NMR chemical shifts are expressed in δ values referring to the solvent peak δC 39.5 for DMSO. Piperonylic acid was purchased from commercial sources (TCI) and used without further purification.
4
Analytical Characterization of Compounds
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Optical rotations were measured on a JASCO P-2300 polarimeter (Tokyo, Japan).1H (500 MHz), and 13C NMR (125 MHz) spectra were recorded on a Bruker 500 NMR spectrometer (USA). The chemical shifts were given in δ (ppm), and coupling constants were reported in Hz. HR-MS spectra were obtained on a JEOL JMS-700 instrument (Tokyo, Japan). Column chromatography (CC) was carried out on polyamide 6L and Sephadex LH 20. Precoated silica gel plates (Merck, Kieselgel 60 F254, 0.25 mm, Merck, Darmstadt, Germany) and precoated RP-18 F254S plates (Merck, Darmstadt, Germany) were used for TLC analysis. A semi-preparative reversed-phase column (Supelco C18 column 250 × 10 mm, 5 μm) was used for HPLC.
5
Characterization of Organic Compounds
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General All chemicals were purchased from TCI (Tokyo, Japan) and used without further purification. Precoated silica gel plates (Merck, Kieselgel 60 F 254 , 0.25 mm) and precoated RP-18 F 254s plates (Merck, Germany) were used for TLC analysis. Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Tokyo, Japan) was used for column chromatography. Melting points were uncorrected. IR spectra (KBr) were recorded on a Nexus670NT Fourier transform (FT)-IR and are reported in frequency of absorption (cm -1 ). High resolution (HR)-FAB-MS and electrospray ionization (ESI)-MS were recorded on JEOL JMS700N and JMS-100TD spectrometers respectively. 1 H-and 13 (link) C-NMR spectra were recorded on a Unity plus 500 spectrometer (Varian Inc., U.S.A.) operating at 500 MHz and referenced to internal residual solvent. NMR data were pro-cessed using the acid citrate dextrose (ACD)/NMR Processor Academic Edition software (Advanced Chemistry Development, Inc., Canada).
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