ESI mass spectra were recorded on a Bruker Esquire 4000 ion trap mass spectrometer connected to a syringe pump for the injection of the samples. The instrument was calibrated using a tune mixture provided by Bruker. Oligosaccharides were dissolved in 50% aqueous methanol -11 mM NH 4 OAc; permethylated oligosaccharides were dissolved in a 1:1 chloroform : methanol mixture, 11mM NH 4 OAc. Samples were injected at 180 μL/h. Detection was performed in the positive ion mode.
Esquire 4000
Manufactured by Bruker
Sourced in Germany, United States
The Esquire 4000 is a high-performance ion trap mass spectrometer designed for a wide range of analytical applications. It features a compact design, high sensitivity, and versatile operation modes to meet the needs of modern analytical laboratories.
Automatically generated - may contain errors
Lab products found in correlation
Agilent 1100 hplc, by Agilent Technologies (2 mentions)
Avance dmx 500 nmr spectrometer, by Bruker (1 mentions)
Spherisorb ods2, by Waters Corporation (1 mentions)
Endo gluc, by Merck Group (1 mentions)
Trypsin, by Merck Group (1 mentions)
5c18 ms 2, by Nacalai Tesque (1 mentions)
Ultimate 3000, by Thermo Fisher Scientific (1 mentions)
V 630, by Jasco (1 mentions)
V 630 spectrophotometer, by Jasco (1 mentions)
16 protocols using esquire 4000
1
ESI-MS Analysis of Oligosaccharides
2
Biotinylated Derivative of Compound 2c
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Briefly, the biotinylated derivative of 2c was obtained by the insertion of a cadaverine linker between biotin and 2c. To this end, biotin was first used to acylate one of the amino groups of cadaverine, and then the resulting adduct was linked to 2c via a carbamate linkage obtained by reaction with 2c-OSu. Products and intermediates were characterized by Electrospray Ionization mass spectrometry (ESI-MS) performed on an Esquire 4000 (Bruker Daltonics) spectrometer and by 1H and 13C NMR (Varian, 500 MHz). Full details are reported in the supplementary materials .
3
ESI-MS Analysis of Flavonoids and Saponins
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ESI–MS analysis was carried out on an Esquire 4000 ion trap mass spectrometer (Bruker–Daltonics, Bremen, Germany) with an electrospray ionization (ESI) interface. The instrument was operated at an ionization voltage of +4000 V and source temperature of 300 °C. Nitrogen was used as nebulizer gas at 30 psi and drying gas at a flow rate of 9 L/min. Collision energy was optimized for each compound. Three time segments were used in mass spectrometric acquisition in order to optimize the instrumental parameters for each compound to increase the peak intensity. The full scan of ions ranging from m/z 100 to m/z 1200 in the negative ion mode was used. Retention times and MS chromatograms of all flavonoids and saponins were confirmed by authentic standards, respectively. The HPLC chromatograms and total ion chromatograms (TIC) were obtained using the above method.
4
NMR and Mass Spectrometry Analysis
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1H NMR (500 MHz) spectra were measured at 25 °C on a Bruker AVANCE DMX 500 NMR spectrometer with TMS as an internal standard. The signals of the residual solvent protons and the solvent carbons were used as internal references. Masses were acquired using an ESI-ion trap detector with positive ionization (Esquire 4000, Bruker Daltonics).
5
HPLC-DAD/MS Analysis of Crude Extract
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The crude extract was re-dissolved in methanol to a concentration of 1.0 mg/mL and subjected to HPLC-DAD/MS using a VWR Hitachi Elite LaChrom system Elite (VWR, Darmstadt, Germany) with an L-2450 diode array detector, an L-2130 pump, and an L-2200 autosampler. This HPLC system was coupled to an ESI-ion trap detector with positive ionization (Esquire 4000, Bruker Daltonics, Faellanden Switzerland) for mass detection. A Onyx Monolithic reversed phase C18 column (100 mm × 3.00 mm; Phenomenex, Torrance, CA, USA) with solvent A (0.1% formic acid in 100% acetonitrile) and solvent B (0.1% formic acid in 100% Milli-Q water) was applied. The gradient parameters were: 0 min 95% A, 4 min 40% A, 6 min 0% A; flow: 2 mL/min).
6
ESI-MS Characterization of Polymer Samples
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The ESI-MS analyses were performed as previously described by Todea et al. [37 (link)]. About 1 mg of crude reaction mixture was dissolved in methanol/acetonitrile (1 mL) and formic acid (0.1% v/v) was added. The analyses were performed using an Esquire 4000 (Bruker) instrument in electrospray positive ionization mode by generating the ions in an acidic environment. The generated ions were positively charged with an m/z ratio that fell in the range of 200–1000. The medium molecular weights, numerical, Mn and gravimetric, Mw and dispersity values, were calculated by using the Equations (1)–(3), as previously reported [65 (link)]:
where Ni is the abundance and Mi is the molecular weight.
where Ni is the abundance and Mi is the molecular weight.
7
HPLC-MS/MS Analysis of Phenolic Compounds
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The analyses were conducted using an Agilent 1100 HPLC (Agilent Technologies Inc., USA) system coupled with an Esquire 4000 ion trap LC/MS system (Bruker Daltoniks, Germany), using a C18 column (5 µm, 4.6 mm i.d x 25 cm, Spherisorb ODS-2, Waters, Ireland). The mobile phase was formic acid in water (0.34% v/v, solvent A) and acetonitrile (solvent B) at a flow rate of 1 mL/min according to the following elution gradient: 0-3 min, 7.3% B; 3-73, 7.3% B; 73-80 min, 35% B; 80-85 min, 70% B; 85-88 min, 70% B; 88-90 min, 7.3%. The total analysis time was 90 min, and 5 min was required for reestablishing and equilibrating the initial conditions. Phenolic compounds were detected at 280 nm. The mass spectral data were acquired in negative mode; ionization (nebulization) was performed with nitrogen as drying gas at 50 psi, 365ºC and at a flow rate of 10 L/min and capillary voltage 3000 V. All scans were performed in the range 50-1400 m/z. The trap parameters were set in ion charge control using manufacturer default parameters. Collision induced dissociation was performed by collisions with the helium background gas present in the trap. Fragmentation was set with Smart Frag.
8
Peptide Analysis by Mass Spectrometry
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The mass spectra of each ACN fraction were performed in a Microflexassisted matrix desorption laser desorption flight time mass spectrometer (Bruker Daltonics Inc., Billerica, MA, USA). The 40% ACN fraction was prepared for ESI MS/MS sequencing. Indeed the extract was reduced (dithiothreitol), alkylated with iodoacetamide and enzymatically digested using trypsin or endo-GluC (Sigma-Aldrich and Promega Corp., Madison, WI, USA) respectively [28] . Proteolysed samples were examined in an LC-MS-MS system consisting of an Agilent 1100 HPLC (Agilent Technologies Inc., Santa Clara, California, USA) coupled to an ESI-TRAP ion trap mass spectrometer Esquire 4000 (Bruker Daltonik GmbH, Bremen, Germany). For Chromatogram Analysis and LC-ESI-MS-MS, Data Analysis Version.
9
ESI Mass Spectrometry of Glycans
10
Chromatographic Separation of Apocarotenoids
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The chromatographic separation of individual apocarotenoids was performed using the Dionex UltiMate 3000 HPLC system equipped with a semi-preparative column (COSMOSIL, 5C18-MS-II, 10 mm internal diameter 3 250 mm) and an Ultimate RS variable-wavelength detector. Mobile phase A (methanol/H 2 O, 9:1 [v/v]) and mobile phase B (100% MTBE) were used as eluent at a flow rate of 3 ml/min. The elution conditions were as follows: 0-20 min 8%-18% B; 20-23 min 18%-50% B; 23-25 min 50%-60% B.
The mass spectrometry identification was performed using an HPLC-DAD-APCI-MS/MS system (Agilent1100, Palo Alto, CA, USA) consisting of an ion-trap mass spectrometer and an APCI ionization source (Esquire 4000; Bruker Daltonics, Bremen, Germany) operated in both negative and positive modes. Nebulizer pressure was set at 60 psi and dry gas (nitrogen) flow was set at 5 l/h. The source temperature was 320 C. The APCI source settings were set as follows: corona discharge voltage, 4000 nA; HV capillary, 3500 V.
The mass spectrometry identification was performed using an HPLC-DAD-APCI-MS/MS system (Agilent1100, Palo Alto, CA, USA) consisting of an ion-trap mass spectrometer and an APCI ionization source (Esquire 4000; Bruker Daltonics, Bremen, Germany) operated in both negative and positive modes. Nebulizer pressure was set at 60 psi and dry gas (nitrogen) flow was set at 5 l/h. The source temperature was 320 C. The APCI source settings were set as follows: corona discharge voltage, 4000 nA; HV capillary, 3500 V.
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