Optical rotations were measured on an Optical Activity AA-55 polarimeter (Optical Activity Ltd., Cambridgeshire, UK). UV spectra were measured on a PuXi TU-1810 UV-visible spectrophotometer (Shanghai Lengguang Technology Co. Ltd., Shanghai, China). ECD spectra were acquired on a JASCO J-715 spectropolarimeter (JASCO, Tokyo, Japan). Quantum chemical calculations were conducted using Gaussian 09 software. NMR spectra were recorded on a Bruker Avance 500 spectrometer (Bruker Biospin Group, Karlsruhe, Germany). Mass spectra were determined on a VG Autospec 3000 or an API QSTAR Pulsar 1 mass spectrometer (VG Instruments, London, UK). HPLC was performed using a Dionex HPLC system (Dionex, Sunnyvale, CA, USA) equipped with a P680 pump, an ASI-100 automated sample injector, and a UVD340U multiple wavelength detector controlled by Chromeleon software (version 6.80). Commercially available Si gel (200-300 mesh, Qingdao Haiyang Chemical Co., Qingdao, China), Lobar LiChroprep RP–18 (40–63 μm, Merck, Darmstadt, Germany), and Sephadex LH–20 (18–110 μm, Merck, Darmstadt, Germany) were used for open column chromatography. Solvents for extraction and purification were distilled prior to use.
Lobar lichroprep rp 18
Manufactured by Merck Group
Sourced in China
Lobar LiChroprep RP-18 is a reversed-phase liquid chromatography sorbent material. It is composed of silica particles with a chemically bonded octadecyl (C18) stationary phase. This sorbent is commonly used for the separation and purification of a wide range of organic compounds in liquid chromatographic applications.
Automatically generated - may contain errors
Lab products found in correlation
Sephadex lh 20, by Merck Group (11 mentions)
Si gel, by Qingdao Haiyang Chemical (6 mentions)
P 1020 digital polarimeter, by Jasco (5 mentions)
J 715 spectropolarimeter, by Jasco (3 mentions)
Xevo g2 xs qtof mass spectrometer, by Waters Corporation (3 mentions)
Hplc system, by Thermo Fisher Scientific (3 mentions)
Chromeleon software version 6, by Thermo Fisher Scientific (3 mentions)
Ltq orbitrap xl spectrometer, by Thermo Fisher Scientific (3 mentions)
Dd2 500 mhz nmr spectrometer, by Agilent Technologies (3 mentions)
Uv 2700 spectrophotometer, by Shimadzu (3 mentions)
Silica gel, by Qingdao Haiyang Chemical (3 mentions)
Agilent dd2 spectrometer, by Agilent Technologies (2 mentions)
Api qstar pulsar 1 mass spectrometer, by Thermo Fisher Scientific (2 mentions)
Asi 100 automated sample injector, by Thermo Fisher Scientific (2 mentions)
Uplc class system, by Waters Corporation (2 mentions)
P680 pump, by Thermo Fisher Scientific (2 mentions)
Uvd340u multiple wavelength detector, by Thermo Fisher Scientific (2 mentions)
J 815 150s circular dichroism spectrometer, by Jasco (2 mentions)
Dionex hplc system, by Thermo Fisher Scientific (1 mentions)
Avance 600 mhz spectrometer, by Bruker (1 mentions)
15 protocols using lobar lichroprep rp 18
1
Comprehensive Analytical Techniques for Compound Characterization
2
Comprehensive Analytical Characterization of Natural Products
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The UV and optical rotations data were obtained on a Shimadzu UV-2700 spectrometer (Shimadzu Co., Ltd., Kyoto, Japan) and Jasco P-1020 automatic polarimeter (JASCO, Tokyo, Japan), respectively. 1H (500 MHz), 13C (125 MHz), and 2D NMR spectra were measured on an Agilent DD2 spectrometer (Agilent Technologies, Waldbronn, Germany). The mass spectra (ESI-MS) were measured under the positive and negative ion modes by a Waters Xevo G2-XS QTof mass spectrometer (Waters, Milford, MA, United States). Column chromatography was performed on silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and on Sephadex LH-20 (Merck). Preparative TLC plates precoated with silica gel GF254 were purchased from Qingdao Marine Chemical Industry Company.
3
Chromatography and Spectroscopic Techniques
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For open column chromatography applications, silica gel of mesh sizes 100–200 and 200–300 (Qingdao Marine Chemical Inc., Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck) were the materials of choice. High-Resolution Electrospray Ionization Mass Spectrometry (HRESIMS) experiments, conducted in positive ion mode, utilized a Waters Xevo G2-XS QTof mass spectrometer (Waters, Milford, MA, United States). Nuclear Magnetic Resonance (NMR) spectroscopic data were collected with a Bruker Avance 600 MHz spectrometer, employing tetramethylsilane (TMS) as an internal standard for calibration. Optical rotations were ascertained utilizing an MCP 500 polarimeter instrument manufactured by Anton Paar. Ultraviolet (UV) spectroscopic analyses were carried out on a Shimadzu UV-1800 spectrometer (Shimadzu Co., Ltd., Kyoto, Japan).
4
Spectroscopic Characterization of Compounds
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UV spectra were measured on a Shimadzu UV-2401PC spectrophotometer (Shimadzu Co. Ltd., Tokyo, Japan). IR spectra were obtained on a Bio-Rad FTS-135 (Bio-Rad, Richmond, Canada) infrared spectrophotometer. The 1D and 2D NMR spectra were obtained at 400 and 100, and 600 and 150 MHz for 1H and 13C, respectively, on Bruker DRX-400 and 600 spectrometers (Bruker, Bremerhaven, Germany) with TMS as an internal standard. MS data were recorded on a VG Autospec-3000 mass spectrometer (VG, Manchester, England). Commercially available silica gel (100−200 mesh or 200−300 mesh, Qingdao Makall Chemical Co. Ltd., Qingdao, China), Lobar LiChroprep RP-18 (40−63 μm, Merck, St. Louis, MO, USA), and Sephadex LH-20 (Pharmacia, Fine Chemical Co. Ltd., Sweden) were used for open-column chromatography. All solvents were distilled prior to use.
5
Comprehensive Analytical Techniques for Chemical Characterization
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Melting points were determined with an SGW X-4 micromeltingpoint apparatus (Shanghai Shenguang Instrument Co. Ltd, Shanghai, China). UV spectra were measured on a PuXi TU-1810 UV-visible spectrophotometer (Shanghai Lengguang Technology Co. Ltd., Shanghai, China). 1D and 2D NMR spectra were obtained at 500 and 125 MHz for 1H and 13C, respectively, on a Bruker Avance 500 MHz spectrometer (Bruker Biospin Group, Karlsruhe, Germany) with tetramethyl silane (TMS) as an internal standard. Mass spectra were generated on a VG Autospec 3000 (VG Instruments, London, UK) or an API QSTAR Pulsar 1 mass spectrometer (Applied Biosystems, Foster, Waltham, MA, USA). Analytical and semipreparative HPLC were performed using a Dionex HPLC system equipped with a P680 pump, an ASI-100 automated sample injector, and a UVD340U multiple wavelength detector controlled by Chromeleon software (version 6.80) (Dionex, Sunnyvale, CA, USA). Commercially available Si gel (200–300 mesh, Qingdao Haiyang Chemical Co., Qingdao, China), Lobar LiChroprep RP-18 (40–63 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Pharmacia, Pittsburgh, PA, USA) were used for open column chromatography. All solvents were distilled prior to use.
6
Chromatographic and Spectroscopic Analysis of Compounds
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Column chromatography was performed with commercially available silica gel (200–300 mesh, Qingdao Haiyang Chemical Co., Qingdao, China), Sephadex LH–20 (American Pharmacia) and Lobar LiChroprep RP–18 (40–63 μm, Merck), notably all solvents were used in their anhydrous forms. Thin-layer chromatography (TLC) plates were carried out using precoated silica gel plates GF254 (Qingdao Haiyang Chemical Factory) and analytical HPLC were performed using a Dionex system equipped with P680 pump, ASI-100 automated sample injector, and UVD340U multiple wavelength detector controlled by Chromeleon software (version 6.80). One-dimensional and two-dimensional NMR spectra were determined at 500 MHz for 1H and 125 MHz for 13C in DMSO-d6, respectively, on a Bruker Avance 500 spectrometer. Low- or high-resolution ESI mass spectra were recorded on a Waters Micromass Q-TOF Premier and a Thermo Fisher Scientific LTQ Orbitrap XL mass spectrometer. The ECD spectra were measured with CH3OH as solvent on a Jasco J-715 spectropolarimeter. Melting points were examined on a SGW X-4 micro-melting-point apparatus. Optical rotations were recorded with a Jasco P-1020 digital polarimeter. UV absorption were evaluated on a Gold S54 Ultraviolet-visible spectrophotometer.
7
NMR and Mass Spectrometry Analysis of AAKLVFF Oligopeptide
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NMR spectra were acquired
on a Bruker AV750 MHz spectrometer using a 5 mm TCI Cryoprobe. Chemical
shifts (δ) were referenced to the MeOH-d4 solvent to provide specific shifts. Oligopeptide AAKLVFF
(purity >98%) was purchased from CSBio (Shanghai) Ltd. The 3 mm
NMR
tubes and MeOH-d4 (purity 99.8%) were
purchased from Deutero GmbH. Mass spectra were recorded on an API
QSTAR Pulsar 1 mass spectrometer (Applied Biosystems, Foster City,
CA). UV spectra were read from a PuXi TU-1810 UV–visible spectrophotometer
(Shanghai Lengguang Technology Co., Ltd., Shanghai, China). Column
chromatography (CC) was used with silica gel (200–300 mesh,
Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep
RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex
LH-20 (18–110 μm, Merck, Germany). Thin layer chromatography
(TLC) was performed with silica gel GF254 precoated plates (100 ×
200 mm, Qingdao Haiyang Chemical Group Corp., Qingdao, China). A separation
and purification experiment was carried out with distilled organic
solvents.
on a Bruker AV750 MHz spectrometer using a 5 mm TCI Cryoprobe. Chemical
shifts (δ) were referenced to the MeOH-d4 solvent to provide specific shifts. Oligopeptide AAKLVFF
(purity >98%) was purchased from CSBio (Shanghai) Ltd. The 3 mm
NMR
tubes and MeOH-d4 (purity 99.8%) were
purchased from Deutero GmbH. Mass spectra were recorded on an API
QSTAR Pulsar 1 mass spectrometer (Applied Biosystems, Foster City,
CA). UV spectra were read from a PuXi TU-1810 UV–visible spectrophotometer
(Shanghai Lengguang Technology Co., Ltd., Shanghai, China). Column
chromatography (CC) was used with silica gel (200–300 mesh,
Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep
RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex
LH-20 (18–110 μm, Merck, Germany). Thin layer chromatography
(TLC) was performed with silica gel GF254 precoated plates (100 ×
200 mm, Qingdao Haiyang Chemical Group Corp., Qingdao, China). A separation
and purification experiment was carried out with distilled organic
solvents.
8
Spectroscopic Characterization of Compounds
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Optical rotations were measured on a P-1020 digital polarimeter (Jasco, Tokyo, Japan) and UV spectra were recorded with MeOH on a UV-2700 spectrophotometer (Shimadzu, Kyoto, Japan). The 1H, 13C, and 2D NMR spectra (500 MHz for 1H and 125 MHz for 13C) were acquired using an DD2 500 MHz NMR spectrometer (Agilent, Santa Clara, CA, USA) with TMS as internal standard. HRESIMS spectra were obtained from a LTQ Orbitrap XL spectrometer (Thermo Scientific, Waltham, MA, USA). Analytical HPLC was performed using a UPLC-class system (Waters, Milford, MA, USA) using a C18 column (1.6 μm, 2.1 mm × 50 mm) equipped with a TUV-detector. Column chromatography (CC) was performed with silica gel (100–200 and 200–300 mesh, Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck). All the solvents purchased were of analytical grade or HPLC grade.
9
Comprehensive Spectroscopic Analysis of Compounds
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NMR spectra were recorded at 500 and 125 MHz for 1H and 13C, respectively, on a Bruker Avance III spectrometer (Bruker, Rheinstetten, Germany). HRESIMS data were determined on a mass spectrometer of Thermo Scientific Orbitrap Fusion Lumos Tribrid (Thermo Scientific, MA, USA) and analyzed using Thermo Xcalibur 4.2 SP1. The circular dichroism (CD) spectrum was acquired on a JASCO J-810 CD spectrometer (JASCO, Tokyo, Japan). Column chromatography (CC) was performed with Silica gel (200–300 mesh; Qingdao Haiyang Chemical Co., Qingdao, China), Lobar LiChroprep RP-18 (40–63 μm; Merck, Kenilworth, NJ, USA), and Sephadex LH–20 (18–110 μm; Merck, Kenilworth, NJ, USA). Semi-preparative HPLC (semi-pHPLC) was performed using a Dionex HPLC system equipped with a P680 pump (flow rate: 3 mL/min), an ASI-100 automated sample injector, and a UVD340U multiple wavelength detector (Detection wavelength: 230 nm) controlled using Chromeleon software, version 6.80 (Dionex Corporation, Sunnyvale, CA, USA).
10
Spectroscopic Characterization of Organic Compounds
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Optical rotations were determined using a Jasco P-1020 digital polarimeter (Jasco, Tokyo, Japan). UV spectra were recorded using a Shimadzu UV-2700 spectrophotometer (Shimadzu, Kyoto, Japan). ECD spectra were obtained with a Jasco J-815-150S circular dichroism spectrometer (Jasco, Inc., Tokyo, Japan). The NMR spectra were recorded using an Agilent DD2 500 MHz NMR spectrometer (500 MHz for 1H and 125 MHz for 13C, Agilent, Santa Clara, CA, USA). HRESIMS data were obtained using an LTQ Orbitrap XL spectrometer (Thermo Scientific, Waltham, MA, USA). Column chromatography was performed using silica gel (200–300 mesh, Qingdao Haiyang Chemical Factory, Qingdao, China), Lobar LiChroprep RP-18 (40–60 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (Merck, Darmstadt, Germany).
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