The peptides were prepared using 9-fluorenylmethyloxycarbonyl (Fmoc) solid-phase synthesis as described previously.45 (link) Briefly, the Fmoc group of H-Rink Amide ChemMatrix resin (0.47 mmol/g) (PCAS BioMatrix) was cleaved with a solution of 6% (wt %) piperidine and 1% (wt %) 1-hydroxybenzotriazole monohydrate (HOBt) in dimethylformamide (DMF) for 20 min and subsequently washed with methanol (MeOH) and dichloromethane (DCM). A coupling solution of Fmoc-protected amino acid (4.0 equiv), tetramethyl-O-(1H-benzotriazol-1-yl) uranium hexafluorophosphate (HBTU) (3.9 equiv), and N,N-diisopropylethylamine (DIEA) (8.0 equiv) was prepared in DMF and incubated with the resin for 90 min. After being washed with MeOH and DCM, the successive Fmoc protecting groups were removed using the same deprotection and washing steps used for the resin, and the progress of the synthesis was periodically verified by electrospray ionization (ESI) mass spectrometry (SCIEX 3200 QTRAP, SCIEX, Framingham, MA). At the end of the solid-phase synthesis, the N-terminal amino acid was acetylated with a solution of acetic anhydride and DIEA in DMF. The peptide was then cleaved from the resin with a solution of 2.5% (vol %) triisopropylsilane and 2.5% (vol %) water in trifluoroacetic acid (TFA) for 2 h and precipitated with cold diethyl ether.
Sciex 3200 qtrap
Manufactured by AB Sciex
Sourced in United States
The SCIEX 3200 QTRAP is a high-performance liquid chromatography-mass spectrometry (LC-MS/MS) system. It combines a triple quadrupole mass analyzer with a linear ion trap, providing enhanced sensitivity and quantitative analysis capabilities. The system is designed for a wide range of applications, including pharmaceutical analysis, environmental monitoring, and food safety testing.
Automatically generated - may contain errors
Lab products found in correlation
Dionex ultimate 3000 lc, by Thermo Fisher Scientific (1 mentions)
Synapt g2 hdms, by Waters Corporation (1 mentions)
1200 series, by Agilent Technologies (1 mentions)
C18 guard column, by Phenomenex (1 mentions)
Agilent 1200 series, by Agilent Technologies (1 mentions)
Kinetex biphenyl column, by Phenomenex (1 mentions)
9 protocols using sciex 3200 qtrap
1
Fmoc Solid-Phase Peptide Synthesis
2
Quantitative Sphingolipid Profiling by LC-MS/MS
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The lipids were extracted from cell pellets (200 µg of protein) by monophasic extraction with water:chloroform:methanol (1:3:6, v/v/v) coupled to alkaline methanolysis. The purified extracts were analyzed by LC Dionex 3000 UltiMate (ThermoFisher Scientific, Waltham, MA, USA) coupled to a tandem mass spectrometer AB Sciex 3200 QTRAP (Sciex, ON, CA). The separation was achieved by reversed-phase chromatography using BEH C8 100 × 2.1 mm × 1.7 μm (Waters, Milford, MA, USA) with a linear gradient between eluent A (0.2% formic acid and 2 mM ammonium formate water solution) and eluent B (methanol, 0.2% formic acid, and 1 mM ammonium formate) [62 (link)]. Mass spectrometry measurement was conducted by multiple reaction monitoring (MRM). The product ion m/z 264 (corresponding to sphingosine) was examined for each precursor ion of ceramides and hexosylceramides, whereas for sphingomyelins, the product ion m/z 184 (corresponding to the choline head) was examined. Specifically, the analysis comprised the sphingolipids, ceramides (Cer, DP 40 eV, and CE 35 eV), hexosylceramides (HexCer, DP 40 eV, and CE 50 eV), and sphingomyelins (SM, DP 40 eV, and CE 50 eV) with fatty acids from C16 to C24. Quantitative analysis was performed using the MultiQuant software (ver 1.2, Sciex, ON, CA).
3
Chlorpyrifos Degradation on SPION@SiO2@TiO2
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Samples (1 mL) were taken for each flask and filtered through a PTFE 0.22 µm filter before analysis. The degradation pathway of chlorpyrifos on SPION@SiO2@TiO2 was studied with HPLC MS/MS (Sciex 3200 Q-trap, Sciex, MA, USA) using a C18 column (Chromolit RP-8e, 4.6 µm × 100 mm, Merck, Darmstadt, Germany). The mobile phase was 80% acetonitrile injected at a flow rate of 0.2 mL·min−1 for 15 min.
4
Preparation and Characterization of Alkoxyamines
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Solvents and
reactants for the
preparation of alkoxyamines were used as received. Routine reaction
monitoring was performed using silica gel 60 F254 TLC plates; spots
were visualized upon exposure to UV light and a phosphomolybdic acid
solution in EtOH, followed by heating. Purifications were performed
on Reveleris X2 Flash System BUCHI switzerland. Cartouches flash Reveleris
and GraceResolv: silica 40 μm. 1H and 13C NMR spectra were recorded in CDCl3, CD3OD,
DMSO-d6 on a 300 or 400 MHz spectrometer.
Chemical shifts (δ) in ppm were reported using residual nondeuterated
solvents as internal references for 1H and 13C NMR spectra. High-resolution mass spectra (HRMS) were obtained
on a SYNAPT G2 HDMS (Waters) spectrometer equipped with a pneumatically
assisted atmospheric pressure ionization source. Positive mode electrospray
ionization was used on samples: electrospray voltage: 2800 V; opening
voltage: 20 V; nebulizer gas pressure (nitrogen): 800 L/h. Low resolution
mass spectra were recorded on the ion trap AB SCIEX 3200 QTRAP equipped
with an electrospray source. The parent ion [M + H]+ is
quoted.
Purity of final compounds was >95% as assessed by
NMR
spectra for all compounds and by HPLC for compound1a .
reactants for the
preparation of alkoxyamines were used as received. Routine reaction
monitoring was performed using silica gel 60 F254 TLC plates; spots
were visualized upon exposure to UV light and a phosphomolybdic acid
solution in EtOH, followed by heating. Purifications were performed
on Reveleris X2 Flash System BUCHI switzerland. Cartouches flash Reveleris
and GraceResolv: silica 40 μm. 1H and 13C NMR spectra were recorded in CDCl3, CD3OD,
DMSO-d6 on a 300 or 400 MHz spectrometer.
Chemical shifts (δ) in ppm were reported using residual nondeuterated
solvents as internal references for 1H and 13C NMR spectra. High-resolution mass spectra (HRMS) were obtained
on a SYNAPT G2 HDMS (Waters) spectrometer equipped with a pneumatically
assisted atmospheric pressure ionization source. Positive mode electrospray
ionization was used on samples: electrospray voltage: 2800 V; opening
voltage: 20 V; nebulizer gas pressure (nitrogen): 800 L/h. Low resolution
mass spectra were recorded on the ion trap AB SCIEX 3200 QTRAP equipped
with an electrospray source. The parent ion [M + H]+ is
quoted.
Purity of final compounds was >95% as assessed by
NMR
spectra for all compounds and by HPLC for compound
5
Dried Blood Spot Alpha-1,4-Glucosidase Activity
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The activity of patient’s alpha-1,4-glucosidase was measured in dried blood spots with NeoLSD™ MSMS kit by ESI-MS/MS using AB SCIEX 3200 Qtrap as described previously [15 (link)].
6
Mass Spectrometry Analysis of Rif Reactions
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Rif (10 μM, in sodium phosphate buffer, pH 7.5) and reaction product samples (collected during HPLC elution) were analyzed with an AB Sciex 3200 Q TRAP mass spectrometry system. The liquid chromatography system was an Agilent 1200 Series. Samples were injected into the mass spectrometer ion source using the flow injection technique. This method employs an Agilent auto-sampler to inject an aliquot from the selected vial into the mass spectrometer without using an HPLC column. The solvent system employed was 50% Barnstead Nanopure water with 0.1% ammonium acetate and 50% methanol. The flow rate was 0.5 mL/min. Electrospray ionization was employed at 4500 volts and a temperature of 600°C. Curtain gas, gas 1, and gas 2 flow pressures were 35, 70, and 60 psi, respectively. Desolvation, entrance, and collision cell entrance potentials were 40, 12, and 22.5 volts, respectively. The mass analyzer system was employed in the Enhanced Mass Spectrum mode, which uses the linear ion trap function, in this case to scan the mass range from 150–1000 Da at a rate of 1000 Da/sec. Mass spectral data was acquired for one minute before another sample was injected.
7
HPLC-MS/MS Quantification of Glycyrrhizin
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Throughout analysis, HPLC and LC-MS/MS working conditions published elsewhere by Cho et al. and validated in the latest publication were employed.6 (link) GTX was analysed using an Agilent 1200 series (HPLC) (Agilent Technologies, Palo Alto, CA, USA) system. Chromatographic separation was performed at +40 °C with a Kinetex biphenyl column (2.6 μm, 100 × 2.1 mm i.d., Phenomenex, Torrance, CA, USA) protected by a C18 guard column (2.1 mmi d.,Phenomenex). Mobile phases consisted of 1% acetic acid in water (A) and 1% acetic acid in methanol (B). Gradient elution procedures were performed under injection with a flow rate of 0–13 min, 5–90% B; 13–20 min 90% B, 0.25 mL/min. The sampler was conserved at below 10 °C and used in a 5-μL injection volume.
Mass spectrometric identification was performed using a Sciex 3200 QTRAP (AB Sciex, Concord, Canada) system in positive ion mode. Analytes were analysed using multıple reactıon monitoring (MRM) in positive ion transfer mode. Ion source temperature was maintained at 600 °C, and the spray voltage was adjusted to 5500 V. All source parameters were optimized under LC conditions, and electrical parameters were optimized with direct infusion. Analist software (version 1.5.1, AB Sciex) was used for device adjustment, data collection and data analysis.
Mass spectrometric identification was performed using a Sciex 3200 QTRAP (AB Sciex, Concord, Canada) system in positive ion mode. Analytes were analysed using multıple reactıon monitoring (MRM) in positive ion transfer mode. Ion source temperature was maintained at 600 °C, and the spray voltage was adjusted to 5500 V. All source parameters were optimized under LC conditions, and electrical parameters were optimized with direct infusion. Analist software (version 1.5.1, AB Sciex) was used for device adjustment, data collection and data analysis.
8
LC-MS/MS Analysis of Pesticides
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The LC-MS/MS method parameters are described in Prado et al. (2020) (link). A liquid chromatograph (LC-Agilent 1200) coupled with a mass spectrometer triple quadrupole (MS/MS QTRAP 3200-SCIEX), with electrospray ionization (ESI) was used for analysis. The column used was a C8 (250 × 4.6 mm, 5 µm, Macherey-Nagel) with a temperature of 25°C using water (A) and acetonitrile (B) acidified with formic acid 0.1%, operating in a gradient mode: 40% (A) for 0.5 min; increasing to 100% in 8 min and kept on this percentage until 12 min; returning to the initial conditions until 12.5 min and kept in this percentage until 18 min. The runtime was 15 min and the retention time of involved analytes was: 9.4 min for difenoconazole and 10.2 min for abamectin.
The method validation was carried according to national and international guidelines (ANVISA 2017; MAPA 2011; SANTE 2017) considering the calibration curves in solvent and matrix (spiked before and after extraction), and the following parameters were evaluated: linearity (the concentration of the analytes varied from 0.5-1000 µg L -1 , containing 10 levels of concentrations in triplicate (n = 3), limits of detection (LOD) and quantification (LOQ), accuracy and precision (3 spiked levels and inter and intra-day injections) and matrix effect.
The method validation was carried according to national and international guidelines (ANVISA 2017; MAPA 2011; SANTE 2017) considering the calibration curves in solvent and matrix (spiked before and after extraction), and the following parameters were evaluated: linearity (the concentration of the analytes varied from 0.5-1000 µg L -1 , containing 10 levels of concentrations in triplicate (n = 3), limits of detection (LOD) and quantification (LOQ), accuracy and precision (3 spiked levels and inter and intra-day injections) and matrix effect.
9
Quantification of Difenoconazole and Abamectin via LC-MS/MS
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The LC-MS/MS method parameters are described in Prado et al. (2020) (link). A liquid chromatograph (LC-Agilent 1200) coupled with a mass spectrometer triple quadrupole (MS/MS QTRAP 3200-SCIEX), with electrospray ionization (ESI) was used for analysis. The column used was a C8 (250 × 4.6 mm, 5 µm, Macherey-Nagel) with a temperature of 25°C using water (A) and acetonitrile (B) acidi ed with formic acid 0.1%, operating in a gradient mode: 40% (A) for 0.5 min; increasing to 100% in 8 min and kept on this percentage until 12 min; returning to the initial conditions until 12.5 min and kept in this percentage until 18 min. The runtime was 15 min and the retention time of involved analytes was: 9.4 min for difenoconazole and 10.2 min for abamectin.
The method validation was carried according to national and international guidelines (ANVISA 2017; MAPA 2011; SANTE 2017) considering the calibration curves in solvent and matrix (spiked before and after extraction), and the following parameters were evaluated: linearity (the concentration of the analytes varied from 0.5-1000 µg L - 1 , containing 10 levels of concentrations in triplicate (n = 3), limits of detection (LOD) and quanti cation (LOQ), accuracy and precision (3 spiked levels and inter and intra-day injections) and matrix effect.
The method validation was carried according to national and international guidelines (ANVISA 2017; MAPA 2011; SANTE 2017) considering the calibration curves in solvent and matrix (spiked before and after extraction), and the following parameters were evaluated: linearity (the concentration of the analytes varied from 0.5-1000 µg L - 1 , containing 10 levels of concentrations in triplicate (n = 3), limits of detection (LOD) and quanti cation (LOQ), accuracy and precision (3 spiked levels and inter and intra-day injections) and matrix effect.
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