Overcoming matrix effects in electrospray: Quantitation of β-agonists in complex matrices by isotope dilution liquid chromatography–mass spectrometry using singly 13C-labeled analogues

González-Antuña, Ana; Domínguez-Romero, Juan C.; García-Reyes, Juan F.; Rodríguez-González, Pablo; Centineo, Giuseppe; Alonso, J. Ignacio García; Molina‐Díaz, Antonio

doi:10.1016/j.chroma.2013.02.074

Cited by 51 publications

(23 citation statements)

References 41 publications

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“…Determination of sludge samples 3.1.1. Clean-up procedure for sludge extracts Quantification analysis of chemicals in complex environmental matrices by LC-(ESI)-MS/MS is often subjected to serious ionization suppression/enhancement by co-eluting compounds [15][16][17][18][19]. And clean-up procedures for the sludge extracts were usually carried out before sample injection [17,20].…”

Section: Resultsmentioning

confidence: 99%

Determination of synthetic phenolic antioxidants and relative metabolites in sewage treatment plant and recipient river by high performance liquid chromatography–electrospray tandem mass spectrometry

Liu

Ruan

Song

et al. 2015

Journal of Chromatography A

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a b s t r a c tRobust analytical methods were developed for the determination of eight emerging synthetic phenolic antioxidants (SPAs) and three metabolites in sewage sludge, effluent and river water matrices. Accelerated solvent extraction was employed for the extraction of the target analytes from sludge, dichloromethane/hexane = 3:1 (extraction solvent) and 90• C (extraction temperature) were used after optimization. Silica gel packed column was chosen for the subsequent cleanup procedure for sludge extract. For the water sample analysis, liquid-liquid extraction combined with silica gel clean-up was used. The targets were determined by optimized high performance liquid chromatography-tandem mass spectrometry method in negative electrospray ionization mode. The method quantification limits of the 11 analytes ranged from 0.1 to 23 ng/L, 0.1 to 20 ng/L and 0.1 to 15 ng/g for sewage effluent, river water and sludge matrices, respectively. The total recoveries of the pretreatment varied from 63 to 106%, with relative standard deviations less than 17% for the three matrices at different spiking levels. Nine targets including 2,6-di-tert-butyl-4-methylphenol (BHT), 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO), 2,6-di-tert-butyl-1,4-benzoquinone (BHT-Q), 2,6-di-tert-butyl-4-hydroxy-4-methyl-2,5-cyclohexadienone (BHT-quinol), 3-tert-butyl-4-hydroxyanisole (BHA), 4-tert-octylphenol (4-tOP), 2,2 -methylenebis(6-tert-butyl-4-methylphenol) (AO 2246), 4,4 -butylidenebis(2-(1,1-dimethylethyl)-5-methyl-phenol) (AO 44B25) and 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene (AO 330) were identified in the collected samples, with concentrations ranging 1.1-2325 ng/g and 0.4-2510 ng/L for sludge and water matrices, respectively. Sewage effluent was considered as a possible contamination source of certain SPA homologues and relative metabolites to the recipient aquatic systems.

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Section: Resultsmentioning

confidence: 99%

Determination of synthetic phenolic antioxidants and relative metabolites in sewage treatment plant and recipient river by high performance liquid chromatography–electrospray tandem mass spectrometry

Liu

Ruan

Song

et al. 2015

Journal of Chromatography A

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“…18,19 It has also been reported that data obtained through the use of the “minimal labeling approach” require corrections by an isotope pattern deconvolution algorithm. 16,17 On the other hand, the limited availability and/or high price of other than d -labeled analogues may be a practical hurdle that prevents their widespread applications.…”

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confidence: 99%

Application of Screening Experimental Designs to Assess Chromatographic Isotope Effect upon Isotope-Coded Derivatization for Quantitative Liquid Chromatography–Mass Spectrometry

2014

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Isotope effect may cause partial chromatographic separation of labeled (heavy) and unlabeled (light) isotopologue pairs. Together with a simultaneous matrix effect, this could lead to unacceptable accuracy in quantitative liquid chromatography–mass spectrometry assays, especially when electrospray ionization is used. Four biologically relevant reactive aldehydes (acrolein, malondialdehyde, 4-hydroxy-2-nonenal, and 4-oxo-2-nonenal) were derivatized with light or heavy (d3-, 13C6-, 15N2-, or 15N4-labeled) 2,4-dinitrophenylhydrazine and used as model compounds to evaluate chromatographic isotope effects. For comprehensive assessment of retention time differences between light/heavy pairs under various gradient reversed-phase liquid chromatography conditions, major chromatographic parameters (stationary phase, mobile phase pH, temperature, organic solvent, and gradient slope) and different isotope labelings were addressed by multiple-factor screening using experimental designs that included both asymmetrical (Addelman) and Plackett–Burman schemes followed by statistical evaluations. Results confirmed that the most effective approach to avoid chromatographic isotope effect is the use of 15N or 13C labeling instead of deuterium labeling, while chromatographic parameters had no general influence. Comparison of the alternate isotope-coded derivatization assay (AIDA) using deuterium versus 15N labeling gave unacceptable differences (>15%) upon quantifying some of the model aldehydes from biological matrixes. On the basis of our results, we recommend the modification of the AIDA protocol by replacing d3-2,4-dinitrophenylhydrazine with 15N- or 13C-labeled derivatizing reagent to avoid possible unfavorable consequences of chromatographic isotope effects.

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“…In addition to the removal of matrix constituents by specific dedicated clean-up protocols and chromatographic separations, other strategies could be simultaneously applied in order to reduce matrix effects to an acceptable level. The most applied approaches are external matrix matched calibration, calibration by standard addition, using analogue internal standard or stable isotopically labelled standards [12,13]. The latter appears to be the most robust and efficient approach [11].…”

Section: Introductionmentioning

confidence: 99%

Accurate determination of selected pesticides in soya beans by liquid chromatography coupled to isotope dilution mass spectrometry

Pérez

Sejerøe-Olsen

Alba

et al. 2015

Talanta

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A sensitive, accurate and simple liquid chromatography coupled with mass spectrometry method for the determination of 10 selected pesticides in soya beans has been developed and validated. The method is intended for use during the characterization of selected pesticides in a reference material. In this process, high accuracy and appropriate uncertainty levels associated to the analytical measurements are of utmost importance. The analytical procedure is based on sample extraction by the use of a modified QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction and subsequent clean-up of the extract with C18, PSA and Florisil. Analytes were separated on a C18 column using gradient elution with water-methanol/2.5 mM ammonium acetate mobile phase, and finally identified and quantified by triple quadrupole mass spectrometry in the multiple reaction monitoring mode (MRM). Reliable and accurate quantification of the analytes was achieved by means of stable isotope-labelled analogues employed as internal standards (IS) and calibration with pure substance solutions containing both, the isotopically labelled and native compounds. Exceptions were made for thiodicarb and malaoxon where the isotopically labelled congeners were not commercially available at the time of analysis. For the quantification of those compounds methomyl-(13)C2(15)N and malathion-D10 were used respectively. The method was validated according to the general principles covered by DG SANCO guidelines. However, validation criteria were set more stringently. Mean recoveries were in the range of 86-103% with RSDs lower than 8.1%. Repeatability and intermediate precision were in the range of 3.9-7.6% and 1.9-8.7% respectively. LODs were theoretically estimated and experimentally confirmed to be in the range 0.001-0.005 mg kg(-1) in the matrix, while LOQs established as the lowest spiking mass fractionation level were in the range 0.01-0.05 mg kg(-1). The method reliably identifies and quantifies the selected pesticides in soya beans at appropriate uncertainty levels, making it suitable for the characterization of candidate reference materials.

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Overcoming matrix effects in electrospray: Quantitation of β-agonists in complex matrices by isotope dilution liquid chromatography–mass spectrometry using singly 13C-labeled analogues

Cited by 51 publications

References 41 publications

Determination of synthetic phenolic antioxidants and relative metabolites in sewage treatment plant and recipient river by high performance liquid chromatography–electrospray tandem mass spectrometry

Determination of synthetic phenolic antioxidants and relative metabolites in sewage treatment plant and recipient river by high performance liquid chromatography–electrospray tandem mass spectrometry

Application of Screening Experimental Designs to Assess Chromatographic Isotope Effect upon Isotope-Coded Derivatization for Quantitative Liquid Chromatography–Mass Spectrometry

Accurate determination of selected pesticides in soya beans by liquid chromatography coupled to isotope dilution mass spectrometry

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