The NMR spectra (1H and 13C) were recorded on four different Bruker instruments including 400 MHz, 500 MHz, 600 MHz, 800 MHz. Chemical shifts are given in δ (ppm) value relative to TMS as internal standard. Deuterated solvents were used to dissolve the samples for NMR experiments. The HR-ESI-MS spectra were obtained from Bruker Compact QToF and MAXIS II mass spectrometers. EI-MS and FAB-MS data were recorded on a Jeol JMS HX 110 mass spectrometer. Silica gel (230–400 meshes) was used for column chromatography. Thin Layer Chromatography (TLC) and preparative TLC were performed on precoated silica gel plates (60 F254, Macherey-Nagel) using various solvent systems as eluent. Spots were visualized using UV light (λmax 254 and 366 nm) and diluted sulphuric acid (10%).
Jms hx 110
Manufactured by JEOL
Sourced in Japan, United States
The JMS HX 110 is a high-resolution magnetic sector mass spectrometer. It is designed for the analysis of a wide range of organic and inorganic compounds, providing accurate mass measurements and high-quality data.
Automatically generated - may contain errors
Lab products found in correlation
Maxis 2, by Bruker (1 mentions)
Compact qtof, by Bruker (1 mentions)
Thin layer chromatography, by Merck Group (1 mentions)
Alpha ftir atr, by Bruker (1 mentions)
Ac 300 500 spectrometers, by Bruker (1 mentions)
Av 600 spectrometer, by Bruker (1 mentions)
B 540 melting, by Büchi (1 mentions)
Nmr spectrophotometer, by Bruker (1 mentions)
α galactosidase, by Merck Group (1 mentions)
Nmr spectrometer, by Bruker (1 mentions)
Dip 360 polarimeter, by Jasco (1 mentions)
Mci gel chp 20p, by Mitsubishi (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
10 protocols using jms hx 110
1
Spectroscopic Characterization of Compounds
2
Characterization of Organic Compounds
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Melting points are determined using a melting-point apparatus (SMP10) in open capillaries and are uncorrected. The progress of the reactions was monitored by thin layer chromatography (Merck). Detections were achieved by UV light illumination. For flash chromatography, commercial silica was used. Nuclear magnetic resonance (1H-NMR, 13C-NMR, and 2D NMR) spectra were determined in DMSO-d6 and were recorded on Bruker AC 300/500 spectrometers using TMS as an internal standard. Chemical shifts are termed in δ (ppm) and coupling constants are described in Hz. The assignment of exchangeable OH and NH was confirmed by D2O. CHNS-microanalysis was done using a Flash EA-1112 instrument. The HREI mass spectra were detected using a Finnigan MAT 95XP. The FAB-MS was done using Jeol JMS HX110. The IR were detected using a Bruker Alpha ATR-FTIR.
3
Comprehensive Spectroscopic Analysis of Organic Compounds
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FT-IR spectra were measured on potassium bromide pellets using an FT-IR spectrophotometer. 1H and 13C NMR/DEPT (90 and 135) spectra (500 MHz and 150 MHz, respectively) and two-dimensional correlation spectroscopy (COSY), NOSEY, HSQC, and HMBC, were recorded in ppm on a Bruker AV-600 spectrometer in CD3OD. Chemical shifts were reported in δ (ppm) values as a solvent and TMS as an internal reference. The molecular weight was determined by positive mode electron ionization mass spectrometry (EI-MS) on a JEOL-MSRoute HX 110 spectrometer. The TOF-ESI-MS was recorded on a JEOL JMS-HX-110 mass spectrometer. Thin layer chromatography (TLC) was carried out on precoated silica gel 60 F254 plates (E. Merck, 0.25 mm), and spots were viewed under UV light (365 and 254 nm) and by spraying with ceric sulfate reagent.
4
Synthesis and Characterization of Novel Compounds
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All the chemicals were purchased from Sigma-Aldrich (Burlington, MA, USA), and commercial-grade solvents were used. Melting points of the synthesized compounds were checked with a Buchi B-540 melting point apparatus (New Castle, DE, USA). A Bruker NMR spectrophotometer (Billerica, MA, USA) was used to attain NMR spectra by using DMSO-d6 and CDCl3 solvents. Mass spectra were generated on a JEOL spectrometer JMS-HX-110 (USA). To monitor the reaction’s progress, TLC on silica gel 60 PF254 cards (Merck, Kenilworth, NJ, USA) was used. UV light (254–365 nm) was used to visualize the product on TLC. For the purification of compounds, silica gel (70–230 mesh) was used in columns.
5
Structural Analysis of Glycolipids
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The structures of the further purified glycolipids were also determined by negative ion fast atom bombardment mass spectrometry (FABMS) and glycosidase treatment. Approximately 5 µg of an isolated neutral glycolipid in 5 µl of chloroform/methanol (1:1, v/v) was mixed with ~5 µl of triethanolamine, and the resultant solution was placed on a stainless steel sample holder for FABMS. Analysis was performed by bombardment with a neutral xenon beam with a kinetic energy of 4 keV, and detection of negative ions was performed with a mass spectrometer (JMSHX-110; JEOL, Ltd., Tokyo, Japan) equipped with a JMA-5500 computer system (JEOL, Ltd.). Assignment of mass numbers was achieved by comparing the spectrum with that of perfluoroalkyl phosphazine (Ultramark 1621; PCR, Inc., Gainesville, FL, USA).
TLC upon treatment with α-galactosidase (Sigma-Aldrich) was performed to confirm the sequence of the sugar chains.
TLC upon treatment with α-galactosidase (Sigma-Aldrich) was performed to confirm the sequence of the sugar chains.
6
Synthesis and Characterization of Novel Compounds
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All the chemicals were sourced from Sigma-Aldrich and Alfa-Aesar. The moisture and air-sensitive reaction were done in an inert environment. The compounds or reaction mixture were dried by a rotary evaporator. The reaction progress was checked by thin-layer chromatography (silica gel 60 PF254 cards) and the reaction mixture was separated through column chromatography by using Silica gel (230–400 mesh). The synthesized compounds were confirmed by spectroscopic analysis, a 500 MHz Bruker NMR spectrometer in the presence of solvent deuterated dimethyl sulfoxide (DMSO-d6). Mass spectra were recorded on a JEOL spectrometer (JMS-HX-110, USA).
7
Spectroscopic Analysis of Isolated Compounds
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The optical rotations ([α]25D) were obtained through a “JASCO DIP 360 polarimeter (Tokyo, Japan)” while the melting points (mps) were measured using “BioCote Stauart SMP10 (Tokyo, Japan)” melting point instrument. The mass spectral assignments were made from EI-MS/HR-EIMS spectra obtained through “JEOL JMS HX 110 (Tokyo, Japan)” while 1H-NMR/13C-NMR spectral measurements were carried out by using “Bruker NMR, Germany (500, 600 MHz for 1H-NMR; 125, 150 MHz for 13C-NMR (δ, ppm)), respectively. FT-IR analyses were determined on “JASCO-320-A spectrophotometer in KBr” as well as “Perkin–Elmer spectrophotometer”. All the solvents used in extraction and isolation of compounds were distilled before use, while the deuterated solvents were used for NMR analysis. Thin layer chromatography (TLC) was carried out using “silica gel F254 pre-coated aluminum sheets”. Visualization of TLC was conducted through a UV lamp at both 254 & 366 nm (λmax) as well as “Dragendorff’s reagent”. The solvent system; 20% acetone-hexane: 10 drops of diethylamine was used as developing solvent for TLC.
8
Comprehensive Spectroscopic Analysis of Compounds
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1D and 2D NMR experiments (1H, 13C, HMQC and HMBC) were recorded on a Jeol EX-500 spectrometer (JOEL Inc., Tokyo, Japan): 500 MHz (1H NMR), 125 MHz (13C NMR). UV spectrophotometer (Shimadzu UV-240), EI-MS: Thermo scientific ISQ spectrometer (70 eV), ESI mass spectra were measured with a JEOL JMS-HX110 instrument. Column chromatography (CC) Polyamide 6S (Riedel-De-Haen AG, Seelze Haen AG, Seelze Hanver, Germany) using MeOH/H2O as eluent. CC Silica gel 60 (Merck, 0.063–0.2 mm) using CH2Cl2:MeOH (2:3). Paper chromatography (PC) (descending) Whatman No. 1 and 3 MM papers, using solvent systems (1) H2O, (2) 15% HOAc (H2O:HOAc 85:15), 3) CAW (CHCl3:HOAc:H2O 90:45:6), (4) BAW (n-BuOH-HOAc-H2O 4:1:5, upper layer), (5) (C6H6:n-BuOH:H2O:pyridine 1:5:3:3, upper layer). Solvents 4 and 5 were used for sugar analysis, Sephadex LH-20 (Pharmazia). Authentic samples were obtained from the department of phytochemistry and plant systematics, NRC. Complete acid hydrolysis for O-glycosides (2 N HCl, 2 h, 100 °C) was carried out and followed by paper co-chromatography with authentic samples to identify the aglycones and sugar moieties.
9
Isolation and Characterization of Bioactive Compounds
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1H, 13C, DEPT, 1H-1H-COSY, HSQC, and HMBC NMR spectra were obtained with a JNM-ECA600 spectrometer. FAB-MS spectra were recorded on a JEOL JMS-HX 110 instrument. The chromatographic stationary phases were silica gel (200-300 mesh), Sephadex LH-20 (25-100 µm, Pharmacia) and MCIgel CHP20P (75-150 mm, Mitsubishi Chemical). Using thin-layer chromatography, compounds were visualized by spraying with 5% H 2 SO 4 , followed by heating (Shen et al. 2013 ).
The ethyl acetate extract was dissolved in ethanol and concentrated in vacuo to yield 11 g oily fraction.
Afterwards, the fraction was subjected to handera-SI (10 µm), and eluted with n-hexane: isopropanol in the range 80:20 - 50:50, to give Fraction 1 (Fr1) 4.
The ethyl acetate extract was dissolved in ethanol and concentrated in vacuo to yield 11 g oily fraction.
Afterwards, the fraction was subjected to handera-SI (10 µm), and eluted with n-hexane: isopropanol in the range 80:20 - 50:50, to give Fraction 1 (Fr1) 4.
10
Comprehensive Phytochemical Analysis by NMR and MS
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General phytochemical analysis methodology 1 H NMR, 13 C NMR and 2D-NMR (COSY, NOESY, HMQC and HMBC experiments) spectra were obtained on a Bruker 600 MHz instrument (Billerica, MA). Homonuclear 1 H connectivities were determined by using the COSY experiment. One bond 1 H- 13 C connectivities were determined with HMQC while two-and threebond 1 H- 13 C connectivities were determined by HMBC experiments, as reported earlier. Chemical shifts were reported in d (ppm) using the solvent (CD 3 OD) standard and coupling constants (J) were measured in Hz. A Jeol JMS HX 110 mass spectrometer (Tokyo, Japan) using glycerol as the matrix was used for mass spectrometry. HREI MS was carried out on Jeol JMS 600 mass spectrometer (Tokyo, Japan). Silica gel 60 (Merck, Darmstadt, Germany) was used as an adsorbent for open column chromatography. TLC analysis was routinely performed using hexane:EtOAc mixtures as the mobile phase and compounds were visualized under UV light.
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