Samples were analyzed by a hybrid quadrupole time-of-flight mass spectrometer (maXis Impact, Bruker Daltonics, Billerica, MA, USA) equipped with an electrospray ionization (ESI) source (drying gas temperature (nitrogen)—180 °C; drying gas flow rate—4 L/min; capillary voltage—4000 V; focusing voltage—500 V; electrospray pressure—0.3 bar; low-pressure funnel RF voltage—90V; high-pressure funnel RF voltage—120 V). The mass spectrometer was set up to prioritize the detection of ions with a mass-to-charge ratio (m/z) ranging from 45 to 900, with a mass accuracy of 1–3 parts per million (ppm). The spectra were recorded in the positive ion charge detection mode. The samples were injected into the ESI source using a glass syringe (Hamilton Bonaduz AG, Bonaduz, Switzerland) connected to a syringe injection pump (KD Scientific, Holliston, MA, USA). The rate of sample flow to the ionization source was 180 µL/h. Mass spectra were obtained using DataAnalysis version 4.1 (Bruker Daltonics) to summarize one-minute signals.
Maxis impact
Manufactured by Bruker
Sourced in Germany, United States
The MaXis impact is a high-performance quadrupole time-of-flight (Q-TOF) mass spectrometer designed for a wide range of analytical applications. It delivers high resolution, accurate mass measurements, and fast data acquisition to support advanced research and development across various industries.
Automatically generated - may contain errors
Lab products found in correlation
Acclaim pepmap c18, by Thermo Fisher Scientific (8 mentions)
Syringe injection pump, by KD Scientific (6 mentions)
Ultimate 3000 rslcnano system, by Thermo Fisher Scientific (6 mentions)
Es tuning mix, by Agilent Technologies (5 mentions)
Compass isotopepattern, by Bruker (4 mentions)
Iraffinity 1, by Shimadzu (4 mentions)
Dataanalysis 4, by Bruker (4 mentions)
Avance 3 hd instrument, by Bruker (3 mentions)
Ultimate 3000, by Thermo Fisher Scientific (3 mentions)
Dataanalysis, by Bruker (2 mentions)
Avance 500 spectrometer, by Bruker (2 mentions)
Dionex ultimate 3000 lc system, by Thermo Fisher Scientific (2 mentions)
Acquity uplc system, by Waters Corporation (2 mentions)
Formic acid, by Merck Group (2 mentions)
Dataanalysis version 4, by Bruker (1 mentions)
Zorbax rrhd sb c18, by Agilent Technologies (1 mentions)
1290 infinity 2, by Agilent Technologies (1 mentions)
Cary 100 bio, by Agilent Technologies (1 mentions)
4 nitrophenol, by Merck Group (1 mentions)
4 nitrobenzoic acid, by Merck Group (1 mentions)
64 protocols using maxis impact
1
Hybrid Quadrupole Time-of-Flight Mass Spectrometry
2
Quantifying Compounds via UPLC-qToF Mass Spectrometry
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Determinations of exact mass were performed on a UPLC system (1290 Infinity II, Agilent, Santa Clara, CA, USA) connected to qToF mass spectrometer (MaXis Impact, Bruker, Billerica, MA, USA). Separation was done with RP-column (Zorbax RRHD SB-C18, 1.8 μm, 2.1 × 100mm, Agilent, Santa Clara, CA, USA). Flow rate was 200 μL/min and the gradient elution of the UPLC with (A) ultra-pure water 0.1% formic acid (B) and acetonitrile was as follows: 0 min: 95% A; 5 min: 95% A; 11 min: 85% A; 22 min: 50% A; 25 min: 20% A; 30 min: 20% A; 35 min: 95% A; 40 min: 95% A. Mass spectrometry parameters in the positive mode were as follows: housing 25 °C, nebulising gas 180 °C, capillary 4500 V. Single ion monitoring (SIM) scanned from 50 to 700 m/z. MS/MS collision energy was 10 eV. Online calibration was done using sodium formate clusters injected at the beginning of each run for 30 s.
3
Spectroscopic Characterization of Nitroaromatic Compounds
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1H and 13C NMR spectra were measured on Bruker
NMR spectrometers working
at 400 and 500 MHz. All of the 13C NMR spectra reported
in this paper are proton-decoupled ones as 13C{1H} spectra. The mass spectra were recorded on maXis impact (Bruker)
using electrospray ionization method. Steady-state fluorescence spectra
were measured on PerkinElmer LS55, and steady-state absorption spectra
were measured on Varian Cary 100 Bio. All of the NACs, given inFigure 2 a, viz., picric acid
(PA), 2,4,6-trinitrotoluene, 1,3-dinitrobenzene (1,3-DNB), 2,4-dinitrotoluene
(2,4-DNT), 4-nitrophenol (4-NP), 3-nitrophenol, 3-nitrotoluene, nitrobenzene
(NB), 4-nitrobenzoic acid, benzoic acid, and methyl benzene or toluene,
were procured from either Sigma-Aldrich or local sources.
NMR spectrometers working
at 400 and 500 MHz. All of the 13C NMR spectra reported
in this paper are proton-decoupled ones as 13C{1H} spectra. The mass spectra were recorded on maXis impact (Bruker)
using electrospray ionization method. Steady-state fluorescence spectra
were measured on PerkinElmer LS55, and steady-state absorption spectra
were measured on Varian Cary 100 Bio. All of the NACs, given in
(PA), 2,4,6-trinitrotoluene, 1,3-dinitrobenzene (1,3-DNB), 2,4-dinitrotoluene
(2,4-DNT), 4-nitrophenol (4-NP), 3-nitrophenol, 3-nitrotoluene, nitrobenzene
(NB), 4-nitrobenzoic acid, benzoic acid, and methyl benzene or toluene,
were procured from either Sigma-Aldrich or local sources.
4
Proteomic Analysis of IgG and PR3-ANCA by nanoLC-MS
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The digested samples were analyzed by nanoLC-reversed phase (RP)-electrospray ionization (ESI) – quadrupole time-of-flight (qTOF)-MS on an Ultimate 3000 HPLC system (Dionex/Thermo Scientific, Sunnyvale, CA) coupled to a MaXis Impact (Bruker Daltonics, Bremen, Germany). The samples were concentrated on a Dionex Acclaim PepMap100 C18 trap column (particle size 5 μm, internal diameter 300 μm, length 5 mm) and separated on an Ascentis Express C18 nano column (2.7 μm HALO fused core particles, internal diameter 75 μm, length 50 mm; Supelco, Bellefonte, PA). The following linear gradient was applied, with solvent A consisting of 0.1% trifluoroacetic acid (TFA; Fluka) and solvent B of 95% acetonitrile (Biosolve, Valkenswaard, The Netherlands): t = 0 min, 3% solvent B; t = 2, 6%; t = 4.5, 18%; t = 5, 30%; t = 7, 30%; t = 8, 1%; t = 10.9, 1%. The sample was ionized in positive ion mode with a CaptiveSprayer (Bruker Daltonics) at 1100 V. A nanoBooster (Bruker Daltonics) was used to enrich the nitrogen gas with acetonitrile to enhance the ionization efficacy. A mass spectrum was acquired every second (frequency of 1 Hz), with the ion detection window set at m/z 550–1800. In between every 12 measurements an external IgG standard was run. A mass spectrum of both total IgG and PR3-ANCA can be seen in Fig. 1 .
5
Characterization of DV1-k-(DV3) Constructs
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A Dionex Ultimate 3000 UPLC System (Thermo Fisher Scientific, Waltham, MA, USA) coupled in series to a UV detector, a 3-inch NaI(Tl) radioactivity detector, and an ultra-high resolution time-of-flight mass spectrometer with electrospray ionization (ESI) (MaXis Impact, Bruker, Bremen, Germany) was used for analysis of all non-radioactive DV1-k-(DV3) constructs. Solvent A (water, 0.1% HCOOH) and solvent B (acetonitrile, 0.1% HCOOH), flow rate 0.6 mL/min, Acquity UPLC BEH C18 1.7 µm 2.1 × 50 mm column (Waters Corporation, Milford, MA, USA). The elution gradient was: 0–2 min: 95% A; 2–10 min: from 95% A to 5% A; 10–12 min: 95% A. UV monitoring of the eluate was performed at 220 nm. For deconvolution analysis of the raw mass spectral data, the software program DataAnalysis (Bruker Daltonik, Bremen, Germany) was used. Calculated average neutral molecular ion mass values were obtained using Compass IsotopePattern (version 3.2, Bruker Daltonik, Bremen, Germany) software.
6
High-resolution mass spectrometry of lipid acylcarnitines
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HRMS was performed on a Bruker maXis impact. The spectrometer parameters were set as follows: ESI (positive ion mode), capillary: 3500 V, end plate offset: −500 V, nebulizer: 0.6 Bar, dry heater: 180 °C, drying gas flow rate: 4.0 L/min. CD-AC was dissolved in methanol (100 μg/mL) and LCA-AC was dissolved in methanol/tetrahydrofuran (100 μg/mL, 9/1 vol.).
7
Tryptic Peptide Separation and Analysis by NanoLC-MS/MS
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NanoLC-MS/MS was performed with a nanoflow ultra-performance liquid chromatography system (UltiMate 3000 RSLCnano system; Dionex) coupled to a hybrid quadrupole time-of-flight (Q-TOF) mass spectrometer (maXis Impact; Bruker). After sample loading, the peptides were eluted frim a trap column into an analytical column (Acclaim PepMap C18, 2 μm, 100 Å, 75 μm × 250 mm; Thermo Scientific) coupled to a nano-electrospray ionization source on the Q-TOF mass spectrometer. A gradient elution of 8% ACN (0.1% FA) to 40% ACN (0.1% FA) over 36 min was used at a flow rate of 300 nL/min for tryptic peptide separation. Eight precursors of charge +2, +3, and +4 from each TOF MS scan were dynamically selected and isolated for MS/MS fragment ion scanning. The MS and MS/MS accumulation were set at 1 and 10 Hz, respectively.
8
Synthesis and Enzyme Inhibition Activity
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UA was supplied by Nanjing Zelang Medical Technology Co., Ltd., with a purity of over 98%. Silica gel (100–200 or 200–300 mesh) used in column chromatography was bought from Tsingtao Marine Chemistry Co., Ltd. Other reagents were purchased from commercial suppliers in their chemically or analytically pure grade without further purification unless otherwise noted.
1H NMR and 13C NMR spectra were recorded on a Bruker AVANCE 400 or Mercury-Plus 300 NMR spectrometers under a standard condition, chemical shifts were measured in ppm downfield from TMS as internal standard (S1 File S2 File 10a , 3b-10b , and 11 were measured on a Bruker maXis impact (S2 File
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1H NMR and 13C NMR spectra were recorded on a Bruker AVANCE 400 or Mercury-Plus 300 NMR spectrometers under a standard condition, chemical shifts were measured in ppm downfield from TMS as internal standard (
9
Mass Spectrometry Analysis of Samples
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Mass spectrometry analysis of the samples was carried out by a hybrid quadrupole time-of-flight mass spectrometer (maXis Impact, Bruker Daltonics, Billerica, MA, USA) equipped with an electrospray ionization (ESI) source. The mass spectrometer was set up to detect ions with the mass-to-charge ratio (m/z) in the range from 50 to 1000 Da and mass accuracy up to 3 parts per million (ppm). The appropriate mass range of the mass spectrometer was previously calibrated by using ES Tuning Mix (Agilent). The spectra were acquired in the positive ion mode detection. The samples were injected into the ESI source using a glass syringe (Hamilton Bonaduz AG, Bonaduz, Switzerland) and a syringe injection pump (KD Scientific, Holliston, MA, USA) with a flow rate of 180 µL/h for 1 min. All samples were analyzed in random order and in two technical replicates.
10
Mass Spectrometry Analysis of Samples
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Samples were analyzed by a hybrid quadrupole time-of-flight mass spectrometer (maXis Impact, Bruker Daltonics, Billerica, MA, USA) equipped with an electrospray ionization (ESI) source. The mass spectrometer was set up to prioritize the detection of ions with a mass-to-charge ratio (m/z) ranging from 45 to 900 Da, with a mass accuracy of 1–3 parts per million (ppm). The spectra were recorded in the positive ion charge detection mode. The samples were injected into the ESI source using a glass syringe (Hamilton Bonaduz AG, Bonaduz, Switzerland) connected to a syringe injection pump (KD Scientific, Holliston, MA, USA). The rate of sample flow to the ionization source was 180 µL/h. Technical replicates were not performed. Mass spectra were obtained using DataAnalysis version 3.4 (Bruker Daltonics, Billerica, MA, USA) to summarize one-minute signals.
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