Premium
Determination of the pesticides diflubenzuron and clofentezine in plums, strawberries and blackcurrant‐based fruit drinks by high performance liquid chromatographic/atmospheric pressure chemical ionization‐mass spectrometry
Author(s) -
Barnes Karen A.,
Fussell Richard J.,
Startin James R.,
Thorpe Stephen A.,
Reynolds Stewart L.
Publication year - 1995
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1290091422
Subject(s) - chemistry , chromatography , atmospheric pressure chemical ionization , diflubenzuron , pesticide , mass spectrometry , chemical ionization , fruit juice , food science , ionization , organic chemistry , ion , agronomy , biology
A high performance liquid chromatographic/atmospheric pressure chemical ionization‐mass spectrometric (HPLC/APCI‐MS) method has been developed for the determination of the pesticides diflubenzuron (1‐(4‐chlorophenyl)‐3‐(2,6‐difluorobenzoyl)urea) and clofentezine (3,6‐bis(2‐chlorophenyl)‐1,2,4,5‐tetrazine) in plums, strawberries and blackcurrant‐based fruit drinks. Samples were homogenized with acetone, extracted into dichloromethane + cyclohexane and cleaned‐up by high performance gel permeation chromatography. HPLC was performed on an ODS column with methanol + water at 1 mL/min. Detection was by negative‐ion selected‐ion monitoring APCI‐MS. Comparison of response with solvent and matrix‐matched standards showed some ehancement of response for the latter, and these standards were consequently used for quantification. The calibration was linear over the range 0.05–0.50 ng/μL in all three matrices. The mean overall recovery of diflubenzuron and clofentezine from spiked extracts (0.086 mg/kg) in all three matrices was 76% and 70% respectively with relative standard deviations of 15% and 12% respectively ( n = 12). The limit of detection was both compound and commodity dependent and ranged from 0.01–0.05 ng/μL, equivalent to 0.003–0.014 mg/kg in the crop.