Multi-class pesticide analysis in human hair by gas chromatography tandem (triple quadrupole) mass spectrometry with solid phase microextraction and liquid injection.

A method for the simultaneous detection and quantification of 22 pesticides from different chemical classes was developed using solid-phase microextraction (SPME) and gas chromatography tandem (triple quadrupole) mass spectrometry. Pesticides were extracted from 50mg of pulverized hair with acetonitrile. The extract was submitted to two successive steps of direct immersion-SPME at 30°C and 90°C or to a liquid injection without SPME in order to obtain optimized conditions for each of the 22 analytes investigated. Validation parameters were significantly influenced by both the injection mode (SPME vs liquid injection) and the temperature of SPME. Limits of quantification ranged from 0.05 pg mg(-1) for trifluralin to 10 pg mg(-1) for pentachlorophenol. The application of the validated method to the analysis of samples collected from non-occupationally exposed volunteers demonstrated the presence of pesticides in all the samples tested. Altogether, 13 different analytes were detected at concentration above the limit of quantification.

[Extraction of trifluralin from acetonitrile solutions].

Results of extraction of trifluralin from an aqueous acetonitrile solution using various organic solvents are presented. The degree of extraction was shown to depend on the nature of extractant and the water/acetonitrile ratio. An optimal electrolyte and the degree of saturation of the water-acetonitrile layer with this electrolyte were selected. The highest efficiency of extraction was achieved by using water-saturated ethylacetate as an extractant. The indices of extraction were calculated as necessary for the isolation of a given amount of trifluralin from aqueous acetonitrile (4:1) solutions with the solvents considered in the present study.

An alternative supercritical fluid extraction system for aqueous matrices and its application in pesticides residue analysis.

Supercritical fluid extraction (SFE) is a rapid and convenient method for the isolation of organic compounds from environmental samples. This paper describes a supercritical carbon dioxide (CO2) extraction system that uses a newly designed extraction cell to recover organic compounds from an aqueous matrix. Analysis of the extracts by gas chromatography-electron capture detector (GC-ECD) indicated that the herbicide trifluralin (2,6-dinitro-N,N-dipropyl-4-trifluoromethylaniline) could be quantitatively extracted by using the SFE system proposed with small amounts of sample. The percentage of recovery obtained with the SFE system described was twice as high as the result obtained using a conventional solid-phase extraction technique. Extraction by SFE was completed in a short period of time using a simple and low-cost home-made system that did not require the use of organic solvents.

Comparison among soil Series and extraction methods for the analysis of trifluralin.

Accurate analytical procedures are needed to improve understanding of the fate and transport of trifluralin, a chemical widely used as a herbicide. Analytical determination of trifluralin is challenging due to its hydrophobic, yet volatile, character and its tendency to degrade into numerous metabolites. In this research, efficient analytical methods for fortified and field-incurred soils were developed for simultaneous quantitation of trifluralin, I [2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)benzenamine, CAS Registry No. 1582-09-8; CAS Registry No. have been provided by the author], a trifluralin metabolite, II [2,6-dinitro-N-propyl-4-(trifluoromethyl)benzenamine, CAS Registry No. 2077-99-8], and a related trifluoromethyldinitroaniline isomer of trifluralin, III [2,4-dinitro-N,N-dipropyl-6-(trifluoromethyl)benzenamine, CAS Registry No. 23106-20-9]. Extractions of trifluralin (0.5 and 2.5 microg/g) from silt loam, sandy loam, and silty clay soils were compared. A method was developed for the supercritical fluid extraction of trifluralin from soil using modified supercritical carbon dioxide, and the effects of cosolvent, pressure, and flow rate on recovery were evaluated. Supercritical fluid extraction was compared to liquid vortex extraction and automated Soxhlet (soxtec) extraction. Solid-phase extraction was examined for purifying soil extracts. Protocols were developed for analysis of extracts by gas and/or liquid chromatography. Immunoassay was investigated but proven to be impractical for this analysis. Soil properties and extraction methods were observed to affect the level of coextracted background interferences. Trifluralin exhibited concentration-dependent recovery regardless of soil series or extraction method.

Adsorption and leaching of trifluralin, metolachlor, and metribuzin in a commerce soil.

Trifluralin [2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)benzenamine], metolachlor [2-chloro-N-ethyl-6-methylphenyl)-N-(2-methoxy-1-methylethyl) aceta mide], and metribuzin [4-amino-6-(1,1-dimethylethyl)-3-(methylthio)-1,2,4,-triazin-5(4H) -one] were selected to study adsorption and leaching potentials related to pollution on Commerce silty clay loam soil near Baton Rouge, Louisiana. At a I:10 soil/water ratio, the Koc values for trifluralin, metolachlor and metribuzin were 875, 135, and 96, respectively. Leaching of these herbicides was evaluated in soil columns (5.4 cm i.d. x 26 cm long). Total recoveries of the herbicides applied to the soil column were 73.1% +/- 4.1%. When the soil columns were leached with three pore volumes of water, the distributions of trifluralin in soil and leachate were 99.993% and 0.007% of the total recoveries, respectively. The distributions of metolachlor was 65.27% in soil and 34.7% in leachate. The distributions of metribuzin was 11.42% in soil and 88.58% in leachate. The results showed that metolachlor and metribuzin were readily leached, while trifluralin was strongly adsorbed to soil. Leaching of three herbicides in the soil column followed the leaching trends of their calculated leaching indices 1.41 x 10(4), 4.18 x 10(6), and 3.38 x 10(8) for trifluralin, metolachlor, and metribuzin, respectively. The results of the study demonstrated the potential of pollution for metolachlor and metribuzin to be leached into the ground water in soils with shallow aquifer.