Determination of carbamate and urea pesticide residues in fresh vegetables using microwave-assisted extraction and liquid chromatography

An analytical multiresidue method for the simultaneous determination of seven pesticides in fresh vegetable samples, namely, courgette (Cucurbita pepo), cucumber (Cucumis sativus), lettuce (Lactuca sativa, Romaine and Iceberg varieties) and peppers (Capsicum sp.) is described. The procedure, based on microwave-assisted extraction (MAE) and analysis by liquid chromatography– photodiode array (LC–PDA) detection was applied to four carbamates (carbofuran, carbaryl, chlorpropham and EPTC) and three urea pesticides (monolinuron, metobromuron and linuron). Extraction solvent and the addition of anhydrous sodium sulphate to fresh vegetable homogenate before MAE were the parameters optimised for each commodity. Recovery studies were performed using spiked samples in the range 250–403 µgkg- 1 in each pesticide. The pesticide residues were extracted using 20mL acetonitrile at 60 ºC, for 10 min. Acceptable recoveries and RSDs were attained (overall average recovery of 77.2% and RSDs are lower than 11%). Detection limits ranged between 5.8 µgkg- 1 for carbaryl to 12.3 µgkg- 1 for carbofuran. The analytical protocol was applied for quality control of 41 fresh vegetable samples bought in Oporto Metropolitan Area (North Portugal). None of the samples contained any detectable amounts of the studied compounds.

Analysis of pesticide residues in strawberries and soils by GC-MS/MS, LC-MS/MS and two-dimensional GC-timeof- flight MS comparing organic and integrated pest management farming

This study analysed 22 strawberry and soil samples after their collection over the course of 2 years to compare the residue profiles from organic farming with integrated pest management practices in Portugal. For sample preparation, we used the citrate-buffered version of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. We applied three different methods for analysis: (1) 27 pesticides were targeted using LC-MS/MS; (2) 143 were targeted using low pressure GC-tandem mass spectrometry (LP-GC-MS/MS); and (3) more than 600 pesticides were screened in a targeted and untargeted approach using comprehensive, two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS). Comparison was made of the analyses using the different methods for the shared samples. The results were similar, thereby providing satisfactory confirmation of both similarly positive and negative findings. No pesticides were found in the organic-farmed samples. In samples from integrated pest management practices, nine pesticides were determined and confirmed to be present, ranging from 2 μg kg−1 for fluazifop-pbutyl to 50 μg kg−1 for fenpropathrin. Concentrations of residues in strawberries were less than European maximum residue limits.

Spent coffee grounds for biodiesel production and other applications

This work evaluates the possibility of using spent coffee grounds (SCG) for biodiesel production and other applications. An experimental study was conducted with different solvents showing that lipid content up to 6 wt% can be obtained from SCG. Results also show that besides biodiesel production, SCG can be used as fertilizer as it is rich in nitrogen, and as solid fuel with higher heating value (HHV) equivalent to some agriculture and wood residues. The extracted lipids were characterized for their properties of acid value, density at 15 °C, viscosity at 40 °C, iodine number, and HHV, which are negatively influenced by water content and solvents used in lipid extraction. Results suggest that for lipids with high free fatty acids (FFA), the best procedure for conversion to biodiesel would be a two-step process of acid esterification followed by alkaline transesterification, instead of a sole step of direct transesterification with acid catalyst. Biodiesel was characterized for its properties of iodine number, acid value, and ester content. Although these quality parameters were not within the limits of NP EN 14214:2009 standard, SCG lipids can be used for biodiesel, blended with higher-quality vegetable oils before transesterification, or the biodiesel produced from SCG can be blended with higher-quality biodiesel or even with fossil diesel, in order to meet the standard requirements.