Journal of Agricultural and Food Chemistry · 2003 · 34 citations · 7 references
PharmacyCrop SciencesChromatographic AnalysisFood AnalysisMass Spectrometric AnalysisAnalytical ChromatographyBioanalytical Method ValidationChromatographyInstrumental AnalysisLiquid ChromatographyMass SpectrometryAnalytical Methods DevelopmentLimit Of Quantification DeterminationLiquid Chromatography-mass SpectrometryLiquid Chromatography-mass Spectrometry AnalysisLiquid Chromatography-mass Spectrometry Method DevelopmentLower Limit Of QuantificationQuantification Limit AnalysisQuantification Limit Assessment
A rapid and sensitive liquid chromatography/electrospray ionization/tandem mass spectrometry (LC-ESI-MS-MS) method has been developed for the determination of the plant growth regulator paclobutrazol in pear samples. Extraction was performed with methanol by using a high-speed blender Ultra-Turrax, and 10 microL of pear extract was directly injected in the LC-ESI-MS-MS system without any previous sample treatment. The highest sensitivity of the method was achieved under MS-MS conditions obtaining a limit of detection of 0.7 microg/kg and a quantification limit of 5 microg/kg, with a run time of only 5.5 min. Recoveries for paclobutrazol from spiked pear samples at 0.005, 0.05, and 0.5 mg/kg were around 82-102% with relative standard deviations between 2 and 7%. The method was applied to real treated and untreated samples of pears, using quality control samples as a evaluation of the method reliability. Two MS-MS transitions were selected, one for quantification (294 > 70) and the other for confirmation of the analyte (296 > 70). All the experiments were performed in compliance with good laboratory practices.
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