Simultaneous screening and quantitative analysis of benzodiazepines by dual-channel gas chromatography using electron-capture and nitrogen—phosphorus detection

Author(s):  
P. Lillsunde ◽  
T. Seppälä
2000 ◽  
Vol 83 (1) ◽  
pp. 178-182 ◽  
Author(s):  
Urania Menkissoglu-Spiroudi ◽  
Grigorios C Diamantidis ◽  
Vassiliki E Georgiou ◽  
Andreas T Thrasyvoulou

Abstract A rapid, reliable, and inexpensive extraction method was developed to determine acaricide residues in honey by gas chromatography (GC) with nitrogen–phosphorus (NP) or electron capture (EC) detectors. Because of the high selectivity of the NP detector, no interfering peaks were present and no cleanup was necessary. A simple cleanup step is proposed for the GC–ECD analysis. Recoveries from spiked honey samples ranged from 79 to 94.4%, with coefficients of variation of 0.3–18.5%. The quantitation limit obtained was 0.015 mg/kg for malathion, 0.020 mg/kg for coumaphos, and 0.005 mg/kg for fluvalinate. The method was used to determine the disappearance of malathion and coumaphos residues from honey samples collected from beehives treated with these acaricides. The disappearance of both acaricides was rapid and followed a first-order model for the duration of the experiment.


1996 ◽  
Vol 79 (6) ◽  
pp. 1423-1427 ◽  
Author(s):  
Rosario Garcia-Repetto ◽  
Isabel Garrtoo ◽  
Manuel Repetto

Abstract A multiresidue analytical method is described for determining 6 pesticides in wine: chlorpyrifos, dimethoate, quinalphos, simazine, tetradifon, and endosulfan. Wine (200 mL) is extracted with dichloromethane (50 mL, 3 times), and the evaporated extracts are purified by silica gel chromatography. Pesticide residues are eluted with n-hexane, n-hexane-benzene (1 + 1), benzene, benzene–acetone (1 + 1), and acetone. Residues are determined by gas chromatography with nitrogen–phosphorus and electron capture detection, using CPSH-5CB, Carbo wax-20M, and CPSH-19CB columns. Recoveries of pesticides added at 0.025 μg/L were 83–97%, with standard deviations of 0.01–0.05%. Detection limits were 0.13–8.9 ng/L, except for simazine (36.7 μg/L). Results are compared with those obtained with a solid-phase extraction (C18) purification and with different eluant series.


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