Step-by-step real time monitoring of a catalytic amination reaction

2019 ◽  
Vol 55 (78) ◽  
pp. 11727-11730 ◽  
Author(s):  
Gilian T. Thomas ◽  
Eric Janusson ◽  
Harmen S. Zijlstra ◽  
J. Scott McIndoe
Keyword(s):  
Real Time ◽  
Multiple Reaction Monitoring ◽  
Reaction Monitoring ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Amination Reaction ◽  
Catalytic Amination ◽  
Multiple Reaction Monitoring Mode ◽  
Sequential Addition ◽  
The Individual

The multiple reaction monitoring mode of a triple quadrupole mass spectrometer is used to examine the Buchwald–Hartwig amination reaction in real-time using sequential addition of reagents to probe the individual steps in the cycle.

Step-by-Step Real Time Monitoring of a Catalytic Amination Reaction

2019 ◽  
Author(s):  
Gilian T. Thomas ◽  
Eric Janusson ◽  
Harmen S. Zijlstra ◽  
J Scott McIndoe
Keyword(s):  
Real Time ◽  
Multiple Reaction Monitoring ◽  
Catalyst Loading ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Amination Reaction ◽  
Catalytic Amination ◽  
Multiple Reaction Monitoring Mode ◽  
Sequential Addition ◽  
The Individual

The multiple reaction monitoring mode of a triple quadrupole mass spectrometer is used to examine the Buchwald-Hartwig amination reaction at 0.1% catalyst loading in real-time using sequential addition of reagents to probe the individual steps in the cycle. This is a powerful new method for probing reactions under realistic conditions.

scholarly journals Step-by-Step Real Time Monitoring of a Catalytic Amination Reaction

2019 ◽  
Author(s):  
Gilian T. Thomas ◽  
Eric Janusson ◽  
Harmen S. Zijlstra ◽  
J Scott McIndoe
Keyword(s):  
Real Time ◽  
Multiple Reaction Monitoring ◽  
Catalyst Loading ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Amination Reaction ◽  
Catalytic Amination ◽  
Multiple Reaction Monitoring Mode ◽  
Sequential Addition ◽  
The Individual

The multiple reaction monitoring mode of a triple quadrupole mass spectrometer is used to examine the Buchwald-Hartwig amination reaction at 0.1% catalyst loading in real-time using sequential addition of reagents to probe the individual steps in the cycle. This is a powerful new method for probing reactions under realistic conditions.

scholarly journals Multiresidue Analysis of Pesticides in Soil by High-Performance Liquid Chromatography with Tandem Mass Spectrometry

2009 ◽  
Vol 92 (5) ◽  
pp. 1566-1575 ◽  
Author(s):  
José Fenoll ◽  
Pilar Hellín ◽  
Carmen M Martnez ◽  
Pilar Flores
Keyword(s):  
High Performance ◽  
Single Phase ◽  
Multiple Reaction Monitoring ◽  
Soil Samples ◽  
Reaction Monitoring ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Multiresidue Analysis ◽  
Multiple Reaction Monitoring Mode

Abstract An analytical multiresidue method using HPLC/MS/MS with a triple-quadrupole mass spectrometer in the multiple reaction monitoring mode for the simultaneous determination of 54 pesticides in soil has been developed. The procedure involved initial single-phase extraction of soil sample with acetonitrile by sonication, followed by liquidliquid partitioning after addition of NaCl. The average recovery by the HPLC/MS/MS method obtained for these compounds varied from 63.2 to 113.8, with an RSD between 1.9 and 7.1. The method gave good linearity over the assay range of 10500 g/L (except famoxadone, 501000 g/L); the LOD and LOQ for the pesticides varied from 0.02 to 13.2 and from 0.1 to 43.9 g/kg, respectively. The proposed method was used to determine pesticide levels in soil samples from two experimental vineyards and two tomato greenhouses.

scholarly journals Determination of Anlotinib, a Tyrosine Kinase Inhibitor, in Rat Plasma by UHPLC-MS/MS and Its Application to a Pharmacokinetic Study

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Zhe Wang ◽  
Le-jing Lian ◽  
Yan-yan Dong ◽  
Xiao Cui ◽  
Jian-chang Qian ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Kinase Inhibitor ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Reaction Monitoring ◽  
Receptor Kinase ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer

Anlotinib is a novel inhibitor of receptor kinase tyrosine with multitargets and has a broad spectrum of inhibitory action on tumor angiogenesis and growth. A simple and rapid UHPLC-MS/MS bioanalytical method was validated for the determination of anlotinib in rat plasma, using imatinib as an internal standard. An Acquity BEH C18 column was used to separate analytes. The eluents consisted of formic acid/water (0.1 : 100, v/v) and acetonitrile with a mobile phase. A triple quadrupole mass spectrometer was operated for the quantification with multiple reaction monitoring (MRM) to determine transitions: 408.2 ⟶ 339.1 for anlotinib, and 494.3 ⟶ 394.1 for imatinib. The validated range was 0.1–50 ng/mL for anlotinib. Mean recovery rate of anlotinib in plasma was ≥99.32% and reproducible. Also, the intra- and interday precisions were both below 15%. This robust method was successfully applied to support the pharmacokinetic study of anlotinib in rats.

scholarly journals Simultaneous Quantification and Pharmacokinetic Study of Five Homologs of Dalbavancin in Rat Plasma Using UHPLC-MS/MS

Molecules ◽  
2020 ◽  
Vol 25 (18) ◽  
pp. 4100
Author(s):  
Difeng Zhu ◽  
Li Ping ◽  
Yawen Hong ◽  
Jiale Shen ◽  
Qinjie Weng ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Pharmacokinetic Analysis ◽  
Pharmacokinetic Studies ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode

Dalbavancin is a novel semisynthetic glycopeptide antibiotic that comprises multiple homologs and isomers of similar polarities. However, pharmacokinetic studies have only analyzed the primary components of dalbavancin, namely B0 and B1. In this study, an ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed to simultaneously determinate and investigate the five homologous components of dalbavancin, namely, A0, A1, B0, B1, and B2, in rat plasma. In this method, methanol was used to precipitate plasma, and a triple-bonded alkyl chromatographic column was used for molecule separation, using 0.1% formic acid-acetonitrile as the mobile phase for gradient elution. Targeted homologs were analyzed by a triple quadrupole mass spectrometer using positive electrospray ionization in multiple reaction monitoring mode. The linearity range was 50–2500 ng/mL with a high correlation coefficient (r2 > 0.998). This method was successfully applied in the pharmacokinetic analysis of dalbavancin hydrochloride to investigate dalbavancin components in rats.

scholarly journals Microdetermination of Emtricitabine in Human Plasma by Liquid Chromatography/Tandem Mass Spectrometry

2009 ◽  
Vol 92 (6) ◽  
pp. 1681-1689 ◽  
Author(s):  
Manish Yadav ◽  
Puran Singhal ◽  
Sailendra Goswami ◽  
Primal Sharma ◽  
Pranav S Shrivastav
Keyword(s):  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reaction Monitoring ◽  
Quadrupole Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Capsule Formulation ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Ion

Abstract A simple, precise, and rapid LC/MS/MS method was developed and validated for the quantification of emtricitabine in human plasma using lamivudine as the internal standard (IS). The method involves liquidliquid extraction of emtricitabine and the IS in diethyl etherethyl acetate (50 + 50, v/v) from 0.1 mL human plasma. A Kromasil C18 (150 4.6 mm, 5 m particle size) analytical column was used for the chromatographic separation under isocratic conditions. The parent product ion transitions for emtricitabine (m/z 248.0130.0) and the IS (m/z 230.1 112.0) were monitored on a triple-quadrupole mass spectrometer, operated in the multiple reaction monitoring positive ion mode. The method was validated over the concentration range of 29.23110 ng/mL for emtricitabine, with a total chromatographic run time of 1.5 min. Acceptable precision and accuracy were obtained for the concentrations used to prepare the standard curves. The applicability of the method was demonstrated by a pharmacokinetic study conducted with 43 healthy volunteers who were administered a capsule formulation containing 200 mg emtricitabine.

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