Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry

In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography-mass spectrometry (GC-MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05-7.0 μg kg−1) with good precision (7.5-20.5%, average 13.7% R.S.D.) and extraction efficiency (69-118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4′-DDE, 4,4′-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.