A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for the first simultaneous identification and quantification of six pyrazole fungicides (furametpyr, rabenzazole, fluxapyroxad, penflufen, bixafen, and isopyrazam) in grape wine samples. The grape wine samples were first diluted with water, then purified by solid-phase extraction, and finally examined by GC-MS/MS in multiple reaction monitoring (MRM) mode. Matrix-matched calibration curves were used to correct the matrix effects. The limits of quantification (LOQs), calculated as 10 times the standard deviation, were 0.2-0.8 μg kg(-1) for the six pyrazole fungicides. The average recoveries were in the range of 74.3-94.5%, with relative standard deviations (RSDs) below 5.8%, measured at three concentration levels. The proposed method is suitable for the simultaneous determination of six pyrazole fungicides in grape wine samples.
Increasing attention has been focused on the artificial flavorings added in foods, especially those for infants and children. For the first time, a sensitive and efficient analytical method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous identification and quantification of four flavoring agents (vanillin, methylvanillin, ethylvanillin, and coumarin) in infant formula samples. The flavorings in samples were extracted with methanol/water (v/v, 1:1), cleaned up by solid-phase extraction, and determined by GC-MS/MS in selected reaction monitoring (SRM) mode. Both isotope-labeled internal standards and matrix-matched calibration solutions were used to correct the matrix effects. The limit of quantification (LOQ) was calculated as 10 times the standard deviation, and it was 10.0 μg kg (-1) for vanillin, methylvanillin, ethylvanillin, and coumarin. The average recoveries were in the range of 82.8-107.5% with relative standard deviations (RSDs) below 8.9% measured at three concentration levels (10, 50, and 100 μg kg(-1)). The proposed method is suitable for the sensitive and accurate simultaneous determination of four flavoring agents in infant formula samples and also provided potential use for reference in terms of real analysis of other foods.
The identification and quantification of four anthocyanins (cyanidin-3-O-glucoside, peonidin-3-O-glucoside, delphinidin-3-O-glucoside, and malvidin-3-O-glucoside) in red grape wine were carried out by hydrophilic interaction liquid chromatography/triple quadrupole linear ion trap MS (HILIC/QTrap-MS/MS). Samples were diluted directly and separated on a Merck ZIC HILIC column with 20 mM ammonium acetate solution-acetonitrile mobile phase. Quantitative data acquisition was carried out in the multiple reaction monitoring mode. Additional identification and confirmation of target compounds were performed using the enhanced product ion mode of the linear ion trap. The LOQs were in the range 0.05-1.0 ng/mL. The average recoveries were in the range 94.6 to 104.5%. The HILIC/QTrap-MS/MS platform offers the best sensitivity and specificity for characterization and quantitative determination of the four anthocyanins in red grape wines and fulfills the quality criteria for routine laboratory application.
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