Analysis of curcumin and calebin-A were performed by using liquid chromatography Thermo–Finnigan surveyor coupled to electrospray ionization on a triple Quad mass spectrometer (Thermo–Finnigan LCQ Advantage Max) equipped with degasser, binary pump, auto sampler, and column heater. For analysis, 4 μl of the extract was injected. The auto sampler was cooled at 10 °C. Chromatographic separation was achieved using C18 column (250 × 4.6 mm, 5μ particle size, Thermo, BDS) with flow rate 0.3 ml/min at 25 °C. The isocratic solvent system was acetonitrile and 0.1% acetic acid in water (40:60). Electrospray ionization was performed in the negative ion mode using helium gas at a pressure of 5 psi for the nebulizer with a flow of 5 l/min and a temperature of 300 °C. The sheath gas temperature was 250 °C with a flow rate of 11 l/min. The capillary was set at 3500 V and the nozzle voltage was 500 V.
Lcq advantage max
Manufactured by Thermo Fisher Scientific
Sourced in United States
The LCQ Advantage MAX is a high-performance liquid chromatography-mass spectrometry (LC-MS) system designed for analytical applications. It provides accurate mass determination and sensitive detection of a wide range of compounds. The system includes a high-resolution quadrupole ion trap mass analyzer and advanced data acquisition capabilities.
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Lab products found in correlation
Cary 50, by Agilent Technologies (2 mentions)
Avance 400 spectrometer, by Bruker (1 mentions)
7890a gc system, by Agilent Technologies (1 mentions)
Hp 5ms chromatographic column, by Agilent Technologies (1 mentions)
5975 c insert 143 xl ei ci msd detector, by Agilent Technologies (1 mentions)
Ultimate 3000 diode array detector, by Thermo Fisher Scientific (1 mentions)
Ultimate 3000 rs autosampler, by Thermo Fisher Scientific (1 mentions)
Ultimate 3000 rs pump, by Thermo Fisher Scientific (1 mentions)
Precoated silica gel plate, by Merck Group (1 mentions)
Avance 300 mhz, by Bruker (1 mentions)
Phospholipase a2, by Merck Group (1 mentions)
Finnigan surveyor plus hplc, by Thermo Fisher Scientific (1 mentions)
Spectrum 100 ft ir, by PerkinElmer (1 mentions)
Cary eclipse, by Agilent Technologies (1 mentions)
Silica gel 60 rp 18, by Merck Group (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Drx 300 spectrometer, by Bruker (1 mentions)
Capcell pak c18 ug120, by Shiseido (1 mentions)
Uv 2450 uv vis spectrophotometer, by Shimadzu (1 mentions)
Agilent 6210 lc tof mass spectrometer, by Agilent Technologies (1 mentions)
17 protocols using lcq advantage max
1
LC-MS Analysis of Curcumin and Calebin-A
2
Mass Spectrometry and NMR Analysis of 3-Methoxymethyl Derivatives
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MS spectra of compounds were recorded on a tandem mass spectrometer Thermo Finnigan LCQ Advantage MAX (USA) in the positive ion [M + H+] mode at an evaporator temperature of 200 °C and capillary temperature of 180 °C. MS/MS spectra were obtained using normalized collision energy (Normolized Collision EnergyTM) ranging from 20 to 40%. Data were collected and processed using the Xcalibur software.
1H- and 13C-NMR spectra were recorded at 400 and 100.6 MHz respectively with a Bruker Avance 400 spectrometer. Chemical shifts were measured relative to tetramethylsilane and solvent signal. Only the characteristic signals in the 1H- and 13C-NMR spectra of 3-methoxymethyl derivatives are shown in Table1 .
1H- and 13C-NMR spectra were recorded at 400 and 100.6 MHz respectively with a Bruker Avance 400 spectrometer. Chemical shifts were measured relative to tetramethylsilane and solvent signal. Only the characteristic signals in the 1H- and 13C-NMR spectra of 3-methoxymethyl derivatives are shown in Table
3
Ion Trap Mass Spectrometry for Spray Analysis
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MS experiments were carried out using a Thermo Finnigan LCQ Advantage MAX ion trap mass spectrometer (San Jose, CA, USA). The main experimental parameters were as follows: spray voltage 0 kV, capillary voltage 4.0 V, tube lens offset –50.0 V, and heated capillary temperature 250 °C. All mass spectra were acquired in positive or negative mode with 3 microscans and were recorded by instrumental software (Xcalibur version 1.4 SR1). The piezoelectric pistol was a generous gift from Prof. R. Graham Cooks and Dr Anyin Li (Purdue University). The pistol was triggered by hand and used to induce spray from the tip end of the hybrid electrode. Each trigger would cause an MS signal to last about 2 seconds. Applied voltage was controlled by a CHI 910B electrochemical workstation (CHI Instruments Inc., TA, USA).
4
Mass Spectrometric Analysis of Compounds
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MS spectra of compounds II , III , and IV were recorded on a tandem mass spectrometer LCQ Advantage MAX (Thermo Finnigan, Waltham, MA, USA) in the positive ion [M + H]+ mode at an evaporator temperature of 350 °C and capillary temperature of 170 °C. MS/MS spectra were obtained using normalized collision energy (Normolized Collision EnergyTM) ranging from 20% to 40%. Data were collected and processed using the Xcalibur software. HRMS experiments for compounds V , VI , VII , and VIII were performed with an Orbitrap Elite mass spectrometer (Thermo Fisher Scientific GmbH, Bremen, Germany) with an ESI source.
1H- and 13C-NMR spectra were recorded at 400 and 100.6 MHz, respectively, with a Bruker Avance 400 spectrometer. Chemical shifts were measured relative to the solvent signal. Only characteristic signals are given in 1H-NMR of steroids.
1H- and 13C-NMR spectra were recorded at 400 and 100.6 MHz, respectively, with a Bruker Avance 400 spectrometer. Chemical shifts were measured relative to the solvent signal. Only characteristic signals are given in 1H-NMR of steroids.
5
Metabolite Extraction from Trichoderma
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Trichloroacetic acid was added to an aliquot of the Trichoderma growth medium (to a concentration of 5%), and then the mixture was centrifuged for 10 min at 10,000× g.
The precipitate was discarded, and metabolites were extracted from the supernatant with ethyl acetate (1:10, v:v). Then, the extract was evaporated, and the residue was dissolved in methanol and analyzed using mass spectrometry.
Mass spectra of the compounds were recorded on an LCQ Advantage MAX quadrupole mass spectrometer (Thermo Finnigan, Bremen, Germany), using a single-channel syringe pump for direct injection of the sample into the chamber for chemical ionization at atmospheric pressure. Detailed information about the structure of compounds was obtained by analyzing MS/MS spectra at the collision energy of 20–40%. Mass spectrometric analysis was carried out by Dr. Baskunov B.P. (IBFM RAS).
The precipitate was discarded, and metabolites were extracted from the supernatant with ethyl acetate (1:10, v:v). Then, the extract was evaporated, and the residue was dissolved in methanol and analyzed using mass spectrometry.
Mass spectra of the compounds were recorded on an LCQ Advantage MAX quadrupole mass spectrometer (Thermo Finnigan, Bremen, Germany), using a single-channel syringe pump for direct injection of the sample into the chamber for chemical ionization at atmospheric pressure. Detailed information about the structure of compounds was obtained by analyzing MS/MS spectra at the collision energy of 20–40%. Mass spectrometric analysis was carried out by Dr. Baskunov B.P. (IBFM RAS).
6
Mass Spectrometry Analysis of Bioactive Compounds
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Fractions C-I were subjected to LC-MS/MS analysis with data collection in data-dependent acquisition mode on a ThermoFinnigan LCQ AdvantageMax mass spectrometer with an electrospray ionization (ESI) source. A Kinetex 5 μm C18 column (100 × 4.6 mm) was used for separation of analytes. The LC method consisted of a linear gradient from 30 to 99% CH3CN in water + 0.1% formic acid over 17 minutes, followed by an isocratic period at 99% CH3CN of 3 minutes. The flow rate was held at 0.6 mL/min. The MS spray voltage was 5 kV with a capillary temperature of 400°C. For the MS/MS component, the CID isolation width was 2.0 and the collision energy was 35.0 eV. The raw data files were converted to mzXML format using MSConvert from the ProteoWizard suite (http://proteowizard.sourceforge.net/tools.shtml )1 . The molecular network was generated using the online platform at Global Natural Products Social Molecular Networking website (gnps.ucsd.edu) using parameters detailed in Table S5 . The network was visualized using the Browser Network Visualizer tool available on the gnps website.
7
Mass Spectrometry Analysis of Compound
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The solution of the examined compound in methanol (0.1 mg/mL) was directly introduced at the rate of 100 µL/ min to the ion source of the ion-trap mass spectrometric system (LCQ Advantage Max; Thermo Finnigan, San Jose, CA, USA). The ESI needle potential was 4.5 kV in the positive ionization mode. The function of secondary ion fragmentation (MS 2 ) was applied for the value at m/z 392. The collision energy was 25%.
8
Lipid and Fatty Acid Quantification in Yeast
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LP was identified and quantified by GC or GC–MS. Dodecane extracts (1 μL) separated from the yeast bi-phase culture, were filtrated and analyzed by GC–MS using an Agilent Technologies 7890A GC system equipped with a 5975C insert 143 XL EI/CI MSD Detector with an HP-5 ms chromatographic column. Helium was used as the carrier gas at a flow rate of 1 mL/min. The oven temperature was kept at 150 °C for 5 min, increased to 250 °C at the rate of 5 °C/min, and finally held at 250 °C for 5 min. The injector and detector temperatures were 250 and 260 °C, respectively. LP amounts were determined using the internal standard 1-eicosene [33 (link)–35 (link)].
Ethyl acetate extracts were analyzed by LC–MS or LC in order to identify and quantify LA. LC–MS was performed on a Thermo Fisher LCQ Advantage MAX instrument equipped with an electrospray ionization detector with a C18 column (4.6 mm × 250 mm). Samples were injected at a column flow of 1 mL/min in the mobile phase (methanol: water: formic acid = 87:13:0.02). LA amounts were determined using standard curves.
Ethyl acetate extracts were analyzed by LC–MS or LC in order to identify and quantify LA. LC–MS was performed on a Thermo Fisher LCQ Advantage MAX instrument equipped with an electrospray ionization detector with a C18 column (4.6 mm × 250 mm). Samples were injected at a column flow of 1 mL/min in the mobile phase (methanol: water: formic acid = 87:13:0.02). LA amounts were determined using standard curves.
9
RNA Analysis by LC-MS
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All RNAs were analyzed on Finnigan LCQ Advantage MAX ion trap instrumentation connected to a Thermo Scientific UHPLC (components: Ultimate 3000 RS Pump, Ultimate 3000 RS Autosampler, Ultimate 3000 RS Column Compartment, Ultimate 3000 Diode Array Detector). RNA mass spectra were acquired in the negative-ion mode with a potential of −4 kV applied to the spray needle (capillary temperature: 270°C, capillary voltage: −2−3 V). LC: 250 pmol RNA dissolved in 30 μl of 20 mM ethylenediaminetetraacetic acid (EDTA) solution; average injection volume: 30 μl; column: Waters xBridge C18 2.5 μm column (1.0 × 50 mm) at 30°C; flow rate: 100 μl/min; eluent A: 8.6 mM triethylamine (TEA), 100 mM 1,1,1,3,3,3-hexafluoroisopropanol in H2O (pH 8.0); eluent B: methanol; gradient: 0–100% B in A within 30 min; UV detection at 260/280 nm. The correct assembly of all RNAs used in this study was confirmed by the mass data.
10
Synthesis of N-Acyl Amide Amphiphiles
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All the essential reagents and solvents needed for the synthesis of N-acyl amides-based amphiphiles were purchased from Alfa Aesar, Sigma Aldrich, Merck, Avra chemicals, Loba, SRL and used as such without any further purification. LR grade solvents and distilled solvents were used when necessary. Thin-layer chromatography using pre-coated silica gel plates purchased from Merck was employed to monitor the reaction progress and visualized by UV detection or p-anisaldehyde stain or molecular iodine. Column chromatography was performed with silica gel (60–120 mesh) purchased from Avra chemicals. 1H- and 13C-NMR spectra for amphiphilic N-acyl amides and their precursors were recorded on a Bruker Avance 300 MHz instrument in CDCl3 at room temperature. Chemical shifts (δ) are reported in parts per million (ppm) using TMS as internal standard and coupling constants (J) are given in Hz. Proton multiplicity is assigned using the following abbreviations: singlet (s), doublet (d), triplet (t), quartet (q), and multiplet (m). Electrospray ionization mass spectra (ESI-MS) were carried out in positive mode with a Thermo Fisher LCQ Advantage Max. instrument by dissolving the solid sample in methanol.
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