Extraction of Pesticides from Plants using Solid Phase Microextraction and QuEChERS

A study employing dispersive solid phase extraction in the formof the quick, easy, cheap, effective, rugged and safe (QuEChERS) method and solid phase microextraction (SPME) for the cleanup of pesticides in plant samples from the Okavango Delta (Botswana) is presented. Concentration levels of aldrin, 1,1-dichloro-2,4-bis[chlorophenyl]ethane (DDD), 1,1-dichloro- 2,2-bis[p-chlorophenyl]ethylene(DDE), 1,1,1-trichloro-2,2-bis[p-chlorophenyl]ethane (DDT), dieldrin, endosulfan and endrin were investigated using gas chromatography with electron capture detection (GC-ECD) and confirmedwith gas chromatography with high resolution time of flight mass spectrometry (GC-TOFMS). Parameters affecting the extraction efficiencies of both techniques were optimized. In the absence of CRMs for the plants under investigation, method validation and evaluation of the extraction efficiencies were achieved through spiking of Nymphaea nouchali (Tswii) leaves at two concentration levels with trichlorobenzene as an internal standard. Recoveries for both SPME and QuEChERS were in the range 61–95 %. The calibration plots were reproducible and linear (R2>0.995) with limits of detection ranging from 0.102 to 1.693 μg L–1 for all the pesticides. The optimal conditions for QuEChERS and SPME were applied to the extraction of pesticides residues from the edible parts (leaves, roots and/ or stems) of Asparagus africanus, Cleome hirta and Nymphaea nouchali plants. No pesticides were detected in the leaves and stems of all the plants studied. Aldrin and endosulfan were detected in the Nymphaea nouchali roots at concentrations of 3–21 μg kg–1 and 5–3 μg kg–1, respectively. Pentachlorobenzene (PCB) and hexachlorobenzene (HCB) were also detected but were not quantified.KEYWORDS Gas chromatography, mass spectrometry, pesticide, plant sample, green techniques

Deltamethrin in sediment samples of the Okavango Delta, Botswana

Deltamethrin concentrations were determined in 35 sediment samples collected from three different habitats: channel, lagoon and pool sites from Xakanaxa in the Okavango Delta, NW Botswana. The samples were Soxhlet-extracted in acetone to extract deltamethrin residues and subsequently cleaned-up with silica gel 60. The final determination was carried out with a gas chromatograph equipped with an electron capture detector (GC-ECD). The sample work-up and determination gave deltamethrin recoveries of 54 to 97%, and detection limits of 0.004 mg/kg dw. The concentration of deltamethrin residues in the sediment samples collected from the three sprayed areas in the Okavango delta ranged between 0.013 and 0.291 mg/kg dw, with the highest concentrations observed in samples obtained from the pool sites. Analysis of samples for organic matter content showed percentage total organic carbon (% TOC) ranging between 0.19% and 8.21%, with samples collected from the pool having the highest total organic carbon. The concentrations of deltamethrin residues and the % TOC in sediment samples showed a similar trend with the highest levels recorded in the pool samples. These data confirmed that a simple method based on GC-ECD, after Soxhlet extraction, was robust enough to enable quantification of deltamethrin in the sediments, because comparable results were obtained with a more sophisticated system consisting of a GC coupled to a mass spectrometer with a time of flight (TOF) analyser. Water SA Vol.32 (4) 2006: pp.483-48