Optimizing microwave-assisted solvent extraction (MASE) of pesticides from soil.

Microwave-assisted solvent extraction (MASE) was investigated as an alternative for extraction of parathion (O,O-diethyl O-4-nitrophenyl phosphorothioate), methyl parathion (O,O-dimethyl O-4-nitrophenyl phosphorothioate), p,p'-DDE [1,1'-dichloro-2,2-bis(4-chlorophenyl)ethane], hexachlorobenzene (HCB), simazine (6-chloro-N2,N4-diethyl- 1 ,3,5-triazine-2,4-diamine) and paraquat dichoride (1,1'-dimethyl-4,4'-bipyridinium) from two different soils and from an earthworm-growing substrate. The matrices were fortified with 14C-radiolabeled pesticides and extracted with various solvent systems under different microwave conditions. Recoveries of more than 80% could be obtained depending on the used microwave conditions and solvent, except for paraquat whose recovery was generally less efficient. Thus, MASE can be successfully used to extract pesticides from environmental and biological samples and could be a viable alternative to conventional extraction methods. The technique uses smaller amounts of organic solvents, thereby minimizing the costs of the analysis and the disposal of waste solvent.

Monitoring of pesticide residues in a cotton crop soil.

This paper reports on the residues of methyl parathion (O,O-dimethyl O-4-nitrophenyl phosphorothioate), trifluralin (alpha, alpha, alpha-trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine), endosulfan [(1, 4, 5, 6, 7, 7-hexachloro-8, 9, 10-trinorborn-5-en-2, 3-ylenebismethylene) sulfite] and dimethoate (O, O-dimethyl S-methylcarbamoylmethyl phosphorodithioate) in a cotton crop soil. Soil samples (0-15 cm) were collected at different periods from the cotton crop farm and subjected to Soxhlet extraction. The extracted material was analysed after clean-up by a HP5890 II gas chromatograph equipped with a 63Ni electron-capture detector (ECD-63Ni) and fitted with a 25 m x 0.2 mm i.d. fused silica capillary column [Ultra-2 (5% phenylmethyl polysiloxane)]. The recoveries of the pesticide residues from the spiked control soil were determined after Soxhlet extraction and C18 cartridges clean-up by using radiotracer techniques with the corresponding 14C-pesticides. The results show that in the cotton crop soil the pesticide residues under study were present in the range of 0.1 to 0.4 mg.kg-1. Endosulfan was found to be rapidly degraded in the soil and formed a sulfate metabolite.

Laboratory tests of the persistence of pesticides in two Brazilian soils.

The persistence of 5 insecticides in two soils, one rich (soil 1), the other poor (soil 2) in organic matter was examined in the laboratory using gas chromatographyc and radiometric techniques. About half DDT and aldrin were lost in 256 days. The other pesticides, in order of decreasing persistence were lindane, parathion (Table I) and malathion (Table II). Aldrin was converted to dieldrin faster in soil 1 than in soil 2. Parathion and lindane were both lost faster from soil 2 than from soil 1. In contrast, malathion was lost more slowly from soil 2 than soil 1, from which all disappeared in 4 days (Table II)

Sorption and movement of pesticides on thin layer plates of Brazilian soils.

The sorption from aqueous solution (Table II), and movement in water on thin layers plates (Figure 1) of 7 soils (Table 1) of 3 organochlorine, 2 organophosphorus and 1 carbamate insecticide was determined in the laboratory. Generally, all substances were sorbed most and moved least on soils richest in organic matter. However, sorption was not a function of organic matter content alone (Table III). Aldrin and DDT were most strongly sorbed and did not move from the point of application on the thin layer plates of any soil. On all 7 soils, carbaryl was the least strongly sorbed insecticide. On 5 soils, lindane, parathion and malathion were increasingly strongly sorbed, but on the other 2 soils lindane was mostly strongly sorbed. The apparent greater mobility of 14C-labelled malathion on thin layers of soils repeatedly leached could be explained by the formation of more polar substances.