ABSTRACT
This work describes the optimization and validation of a method employing solid-liquid extraction with low temperature partitioning (SLE/LTP) together with analysis by gas chromatography with electron capture detection (GC/ECD) for the determination of nine pesticides (chlorothalonil, methyl parathion, procymidone, endosulfan, iprodione, λ-cyhalothrin, permethrin, cypermethrin, and deltamethrin) in lettuce. The method was found to be selective, accurate, and precise, with means recovery values in the range of 72.3-103.2%, coefficients of variation ⩽ 12%, and detection limits in the range 0.4-37 µg kg(-1). The matrix components significantly influence the chromatographic response of the analytes (above 10%). The optimized and validated method was applied to determine the residual concentrations of the fungicides iprodione and procymidone that had been applied to field crops of lettuce. The maximum residual concentrations of the pesticides in the lettuce samples were 13.6 ± 0.4 mg kg(-1) (iprodione) and 1.00 ± 0.01 mg kg(-1) (procymidone), on the day after application of the products.
Subject(s)
Chromatography, Gas/methods , Lactuca/chemistry , Pesticide Residues/isolation & purification , Solid Phase Extraction/methods , Food Contamination/analysis , Methyl Parathion/analysis , Methyl Parathion/isolation & purification , Nitriles/analysis , Nitriles/isolation & purification , Pesticide Residues/analysis , Pyrethrins/analysis , Pyrethrins/isolation & purification , TemperatureABSTRACT
A method has been optimized and validated for the determination of fomesafen in soils using solid-liquid extraction with low-temperature partitioning (SLE/LTP) and analysis by liquid chromatography with a high-efficiency diode array detector (HPLC/DAD). The method was used to evaluate the persistence and mobility of this herbicide in different soils cultivated with bean plants. Recovery values were ≥98.9 %, with variations in the repeatability coefficients of ≤15 %, and a detection limit of 7.3 µg kg(-1). Half-life values of fomesafen were between 60 and 71 days in soil cultivated using a no-till system and 99 and 114 days in soil cultivated using a conventional tillage system. The mobility of fomesafen was moderate and mainly influenced by the organic matter content, pH, and soil type. In Red-Yellow Argisol, which has a higher content of organic matter, the leaching of fomesafen was less pronounced. In Red-Yellow Latosol, which has smaller amounts of organic matter and high pH, the leaching of fomesafen was more pronounced.
