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Interest in the determination and screening of pesticide residues in soil is caused by widespread use of chemical pesticides in agriculture, which increase soil contamination. Two extraction techniques, matrix solid phase dispersion (MSPD) and liquid-liquid extraction (LLE) of residual pesticides (acaricides, insecticides, herbicides, and fungicides) from soil were compared. Advantages and disadvantages of both approaches were discussed. Pesticides from different chemical classes (organohalogen, organophosphorus, carbamates, pyrethroids, strobilurines, triazoles) were quantified by GC with a dual system detection - electron capture (EC) and/or nitrogen-phosphorus (NP). The MSPD was validated by comparing it with conventional LLE. Recovery studies were carried out at three levels: 1) ranged between 0.005-0.05 mg/kg, 2) 0.05-0.5 mg/kg, and 3) 0.25-2.5 mg/kg and average recoveries obtained for these compounds ranged from 72.4 to 120% for MSPD and 70.6-120% for LLE with relative standard deviations (RSDs) below 20%. Both methods were linear over the range assayed, 0.005-2.5 mg/kg. The uncertainties of the analytical methods were lower than 25.6% and 30%, with and without recovery correction, respectively. The rapid and practical MSPD technique has found a particular application in determining 147 pesticide residues of different physicochemical properties in soil with satisfactory validation parameters. The study estimated that MSPD has significant advantages over LLE because, coupled with simultaneous stage of purification, it allowed for a radical reduction time of analysis and its cost. MSPD fulfilled the requirements of multiresidue techniques. The method is reliable and can be useful for routine monitoring in soil.
The resistance of edible oils to oxidative degradation, leading to rancidification, is an important parameter for assessing the quality of oil. This paper presents a new promising method to diagnose the volatile compounds which are products of oil oxidation reactions. Our experiment was carried out using a combined method of UV irradiation as an oxidation acceleration technique, headspace solid-phase microextraction (HS-SPME) as an extraction technique and capillary gas chromatography (GC) as an assay technique. Method precision and sensitivity expressed as RSD (<19%) and LOD (between 18 and173 ng/mL) are satisfactory. The induction period set on hexanal / t-2-nonenal ratio (IP=6.67 h) is comparable with those obtained with the Rancimat method (4.64–6.73 h).
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