Ion Spray Mass Spectrometry for Elemental Speciation in Aqueous Samples: Preliminary Investigation of Experimental Parameters, Matrix Effects and Metal–Ligand Complexation

1997 ◽  
Vol 12 (5) ◽  
pp. 507-515 ◽  
Author(s):  
JOHN W. OLESIK ◽  
KURT K. THAXTON ◽  
SUSAN V. OLESIK
Keyword(s):  
Mass Spectrometry ◽  
Matrix Effects ◽  
Preliminary Investigation ◽  
Elemental Speciation ◽  
Aqueous Samples ◽  
Experimental Parameters ◽  
Ion Spray Mass Spectrometry ◽  
Metal Ligand

scholarly journals Analytical Methods for Quantification and Identification of Intact Glucosinolates in Arabidopsis Roots Using LC-QqQ(LIT)-MS/MS

Metabolites ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 47
Author(s):  
Kourosh Hooshmand ◽  
Inge S. Fomsgaard
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Crude Extract ◽  
Matrix Effects ◽  
Critical Role ◽  
Reversed Phase ◽  
Biologically Active ◽  
Natural Soil ◽  
Chromatography Method ◽  
Arabidopsis Root

Glucosinolates are biologically active secondary metabolites in Brassicaceae plants that play a critical role in positive and negative interactions between plants and root-associated microbial communities. The aim of this study was to develop a reversed-phase liquid chromatography method to quantify and identify intact glucosinolates in the root of Arabidopsis thaliana (Arabidopsis) grown in non-sterile natural soil by using liquid chromatography-hybrid triple quadruple-linear ion trap (LC-QqQ(LIT)) mass spectrometry. The Synergi Fusion C18-based column was found to be effective for sufficient retention and separation of nine intact glucosinolates without the need for time-consuming desulfation or ion-pairing steps. Method validation results showed satisfactory inter-day and intra-day precision for all glucosinolates except for 4-hydroxyglucobrassicin. Good inter-day and intra-day accuracy and recovery results were observed for glucoiberin, gluconapin, glucobrassicin, 4-methoxyglucobrassicin and neoglucobrassicin. However, for 4-hydroxyglucobrassicin, glucoraphanin and glucoerucin corrections to quantification results might be necessary since the recovery and accuracy results were not optimal. Matrix effects were shown to have a negligible effect on the ionization of all target analytes. The established liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was applied to quantify target intact glucosinolates in Arabidopsis root crude extract of four different wild-type accessions where differences in terms of concentration and composition of intact glucosinolates were observed. Employment of sensitive and selective precursor ion survey scan of m/z 97 in combination with the information-dependent acquisition (IDA) of the enhanced product ion (EPI) dependent scan (Prec97-IDA-EPI) using LC-QqQ(LIT) provided high confidence in structural characterization of diverse intact glucosinolate profiles in complex Arabidopsis root crude extract.

scholarly journals Characterization and Study on Fragmentation Pathways of a Novel Nerve Agent, ‘Novichok (A234)’, in Aqueous Solution by Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 1059
Author(s):  
Jin Young Lee ◽  
Kyoung Chan Lim ◽  
Hyun Suk Kim
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Solution ◽  
Liquid Chromatography ◽  
Degradation Products ◽  
Aqueous Sample ◽  
Tandem Mass ◽  
Aqueous Samples ◽  
Fragmentation Pathways ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

As a first step toward studying the properties of Novichok (ethyl (1-(diethylamino)ethylidene)phosphoramidofluoridate (A234)), we investigated its degradation products and fragmentation pathways in aqueous solution at different pH levels by liquid chromatography–tandem mass spectrometry. A234 was synthesized in our laboratory and characterized by nuclear magnetic resonance spectroscopy. Three sets of aqueous samples were prepared at different pH levels. A stock solution of A234 was prepared in acetonitrile at a concentration of 1 mg/mL and stored at −20 °C until use. Aqueous samples (0.1 mg/mL) were prepared by diluting the stock solution with deionized water. The acidic aqueous sample (pH = 3.5) and basic aqueous sample (pH = 9.4) were prepared using 0.01 M acetic acid and 0.01 M potassium carbonate, respectively. The analysis of the fragmentation patterns and degradation pathways of A234 showed that the same degradation products were formed at all pH levels. However, the hydrolysis rate of A234 was fastest under acidic conditions. In all three conditions, the fragmentation pattern and the major degradation product of A234 were determined. This information will be applicable to studies regarding the decontamination of Novichok and the trace analysis of its degradation products in various environmental matrices.

scholarly journals Multi-residue analytical methods for the determination of pesticides and PPCPs in water by LC-MS/MS: a review

2012 ◽  
Vol 10 (3) ◽  
pp. 876-899 ◽  
Author(s):  
Ednei Primel ◽  
Sergiane Caldas ◽  
Ana Escarrone
Keyword(s):  
Mass Spectrometry ◽  
Analytical Methods ◽  
Environmental Samples ◽  
World Wide ◽  
Matrix Effects ◽  
Tandem Mass ◽  
Selective Determination ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractResidues of pesticides, pharmaceutical and personal care products (PPCPs) are contaminants of world-wide concern. Consequently, there is a growing need to develop reliable analytical methods, which enable rapid, sensitive and selective determination of these pollutants in environmental samples, at trace levels. In this paper, a review of the liquid chromatography-tandem mass spectrometry (LC-MS/MS) based methods for the determination of pesticides and PPCPs in the environment is presented. Advanced aspects of current LC-MS/MS methodology, including sample preparation and matrix effects, are discussed.

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