Search results for "Reaction Monitoring"
showing 6 items of 26 documents
Determination of ketosteroid hormones in meat by liquid chromatography tandem mass spectrometry and derivatization chemistry.
2015
A method for the determination and quantification of ketosteroid hormones in meat by mass spectrometry, based on the derivatization of the carbonyl moiety of steroids by O-methylhydroxylamine, is presented. The quantitative assay is performed by means of multiple-reaction-monitoring (MRM) scan mode and using the corresponding labelled species, obtained by reaction with d 3-methoxylamine, as internal standard. The accuracy of the method was established by evaluating artificially spiked samples, obtaining values in the range 90-110%. Recovery tests were performed on blank matrix samples spiked with non-natural steroids including trenbolone and melengestrol acetate. The latter experiment revea…
Reproducible and Consistent Quantification of the Saccharomyces cerevisiae Proteome by SWATH-mass spectrometry *
2015
Targeted mass spectrometry by selected reaction monitoring (S/MRM) has proven to be a suitable technique for the consistent and reproducible quantification of proteins across multiple biological samples and a wide dynamic range. This performance profile is an important prerequisite for systems biology and biomedical research. However, the method is limited to the measurements of a few hundred peptides per LC-MS analysis. Recently, we introduced SWATH-MS, a combination of data independent acquisition and targeted data analysis that vastly extends the number of peptides/proteins quantified per sample, while maintaining the favorable performance profile of S/MRM. Here we applied the SWATH-MS t…
Pressurized liquid extraction combined with capillary electrophoresis–mass spectrometry as an improved methodology for the determination of sulfonami…
2007
A new analytical method, based on capillary electrophoresis and tandem mass spectrometry (CE-MS2), is proposed and validated for the identification and simultaneous quantification of 12 sulfonamides (SAs) in pork meat. The studied SAs include sulfathiazole, sulfadiazine, sulfamethoxypyridazine, sulfaguanidine, sulfanilamide, sulfadimethoxyne, sulfapyridine, sulfachloropyridazine, sulfisoxazole, sulfasalazine, sulfabenzamide and sulfadimidine. Different parameters (i.e. separation buffer, sheath liquid, electrospray conditions) were optimized to obtain an adequate CE separation and high MS sensitivity. MS2 experiments using an ion trap as analyzer, operating in the selected reaction monitori…
Evaluation of enniatins A, A1, B, B1 and beauvericin in Portuguese cereal-based foods.
2012
Sixty-one samples of Portuguese cereal-based foods were analysed for the occurrence of emerging mycotoxins called enniatins (A, A1, B and B1) and beauvericin. Samples were extracted with a mixture of acetonitrile/water (85/15, v/v) using an Ultra-Turrax homogeniser, and mycotoxins were detected with liquid chromatography coupled to a mass spectrometer. This method was validated and adequate values of recovery (70-103%) and relative standard deviation (15%) were obtained. Signal suppression/enhancement was studied and matrix-matched calibration used to minimise this effect, but no additional clean-up step was necessary. The mass spectrometer was operated in selected reaction monitoring (SRM)…
Multiple reaction monitoring for identification and quantification of oligosaccharides in legumes using a triple quadrupole mass spectrometer.
2022
Raffinose family oligosaccharides are non-digestible compounds considered as dietary prebiotics with health-related properties. Hence, it is important to develop highly specific methods for their determination. An analytical method is developed in this study for oligosaccharide identification and quantification using liquid chromatography-tandem mass spectrometry equipped with a triple quadrupole analyser operating in Multiple Reaction Monitoring mode. Raffinose, stachyose and verbascose are separated in a 10-minute run and the method is validated over a broad concentration range, showing good linearity, accuracy, precision and high sensitivity. A low-cost, short eco-friendly procedure for …
Determination of aminoglycoside and macrolide antibiotics in meat by pressurized liquid extraction and LC-ESI-MS
2010
A simple method for the simultaneous determination of dihydrostreptomycin, spectinomycin, spiramycin, streptomycin, tilmicosin, and tylosin in meat has been developed using pressurized liquid extraction and LC-triple quadrupole MS (LC-ESI-MS/MS). The pressurized liquid extraction operational parameters were optimized and no protein precipitating and fat removing steps were required. A gradient HPLC separation was developed with ion-pair mobile phases consisting of aqueous 1 mM heptafluorobutyric acid water and methanol. Protonated molecules were used as precursor ions for CID. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring of three fragment ion transition…