Analysis of diclofenac in water samples using in situ derivatization-vortex-assisted liquid-liquid microextraction with gas chromatography-mass spectrometry.

A novel micro-extraction technique for a rapid and sensitive analysis of diclofenac (DCF) in water samples has been developed. DCF was derivatized and extracted simultaneously using vortex-assisted liquid-liquid micro-extraction (VALLME) prior to gas chromatography with mass spectrometry detection. The effects of extraction solvent volume, extraction and derivatization time and ionic strength of the sample were studied using 23 factorial experimental design. The optimum extraction conditions were as follows: 200 µL of chloroform, 25 µL of N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) derivatization reagent, vortex extraction and derivatization time 5 min at 3000 rpm. The extraction recovery for different fortification levels was 98 %. Also, the proposed micro-extraction method exhibited results comparable with the solid phase extraction of real water samples. The proposed one-step VALLME and derivatization method is simpler and faster than the conventional extraction and derivatization methods used for the determination of DCF in real water samples.

Effects of long-term irrigation with untreated municipal wastewater on soil properties and crop quality.

Irrigating crops with untreated wastewater leads to elevated concentrations of heavy metals both in soil and cultivated crops. The current study was designed to determine heavy metal (i.e., Pb, Cd, Cr, Cu, Ni, Zn, Hg) accumulation in Konya soils in selected nine sites irrigated with wastewater for over 40 years. Non-irrigated soil samples and soil samples irrigated with well water were taken as control samples. Transport of these pollutants to the wheat samples cultivated in the investigated site was also examined. The obtained results reveal that high alkaline properties and clay structure of Konya soil reduce the mobility of contaminants and cause accumulation in the top layer of soil. Intense effect of wastewater irrigation on soil EC was determined. The highest concentrations of Pb, Cr, Cu, Cd, Zn, Ni, and Hg in wastewater irrigated soil were 5.32, 37.1, 31.5, 11.4, 91.5, 134, and 0.34 mg kg(-1), respectively. Wastewater irrigated soils were strongly polluted by means of Cd (8.23-11.6 mg kg(-1)) and moderately to strongly polluted by means of Ni (47.7-134 mg kg(-1)), exceeding Maximum Admissible Concentrations for Trace Elements in Agricultural Soils and Sewage Sludge Regulation limit values of Turkey. Maximum concentrations found for Pb, Cr, Cu, Cd, Zn, and Ni in wastewater irrigated wheat grain were 8.44, 1.30, 9.10, n.d, 29.31, and 0.94 mg kg(-1), respectively. Besides, Hg was not detected in any samples of wheat grain. Based on the regulation of Turkish Food Codex, Pb contamination in wheat samples grown in the sampling site was evidenced.