Determination of the Pesticide Fenbutatin Oxide in Tomatoes, Cucumbers and Bananas by High Performance Liquid Chromatographic/Atmospheric Pressure Chemical Ionization-Mass Spectrometry

✍ Scribed by Karen A. Barnes; Richard J. Fussell; James R. Startin; Hilary J. Mobbs; Richard James; Stewart L. Reynolds

• Publisher: John Wiley and Sons
• Year: 1997
• Tongue: English
• Weight: 156 KB
• Volume: 11
• Category: Article
• ISSN: 0951-4198
• DOI: 10.1002/(sici)1097-0231(19970131)11:2<159::aid-rcm730>3.0.co;2-o

✦ Synopsis

A rapid method, using high-performance liquid chromatography (HPLC)/atmospheric pressure chemical ionization-mass spectrometry, has been developed for the determination of fenbutatin oxide in tomatoes, cucumbers and bananas. Samples were homogenized with sodium carbonate and ethyl acetate, filtered through sodium sulphate, concentrated and solvent exchanged into acetonitrile prior to analysis. HPLC was performed on a Hypercarb column with 10:90 acetic acid (5% v/v glacial acetic acid in water)/acetonitrile at a flow rate of 1 mL/min. Positive ionization selected-ion monitoring was performed on the 7 isotopic cluster ions from the tris(2-methyl-2-phenylpropyl) tin fragment. A comparison of solvent-based and extract-based standards showed that tomato and cucumber matrices had a slight enhancement effect on the signal intensity, whereas the banana matrix exerted a signal suppression effect. Calibration was linear over the range 0.25-5.0 ng/µL. The mean spike recoveries (extracts spiked at 0.5 mg/kg) were 88% for tomatoes and 80% for both cucumbers and bananas with relative standard deviations of 6%, 7% and 8% respectively. Limits of detection were commodity dependent and ranged from 0.06-0.12 ng/µL (equivalent to 0.01-0.02 mg/kg in the crop). Ionization was stable for long analytical time periods.