Simultaneous multi-residue pesticide analysis in southern Brazilian soil based on chemometric tools and QuEChERS-LC-DAD/FLD method

Pesticide-Residue Analysis in Soils by the QuEChERS Method: A Review

“…The QuEChERS method was the most efficient extraction procedure: around 50% of the 24 multiclass pesticides analyzed had recoveries satisfying the 70-120% recovery range and a median recovery of 72.7%. Table 1 summarizes a representative sample of the subsequent studies regarding the QuEChERS extraction approaches for the analysis of a wide range of pesticide residues belonging to different chemical families, such as organochlorine pesticides (OCPs) [15,16,20,25,29,48], organophosphorus pesticides (OPPs) [25], pyrethroid pesticides (PYPs) [25,47], neonicotinoids [35,57], carbamates [53], and triazole [18] and urea [22] derivatives, among others. Depending on the country, the types of pesticides vary due to the characteristic crops of each geographical and climatic zone.…”

“…In some cases, ultra-high-performance liquid chromatography (UHPLC) coupled with MS/MS was employed for high throughput, especially when hundreds of pesticides were analyzed simultaneously [49,50]. Less sensitive techniques for pesticide residue analysis in soil samples include HPLC with traditional detectors, such as diode array detectors (DADs) [17,35], fluorescence detectors (FLDs) [53], ultraviolet (UV) [52] and GC with electron-capture detectors (ECDs) [16,25,29,36], and nitrogen phosphorous detectors (NPDs) [36] or flame photometric detectors (FPDs) [25] for OCPs and OPPs, respectively. In this context, Łozowicka et al [36] studied the extent and variability of the matrix effects of pesticides using GC with different types of detectors (MS/MS and µECD/NPD).…”

“…In this context, different sample amounts have been extracted after proper homogenization through mechanical processes, such as grinding and sieving. Methods involving 1 g [53], 2 g [20], 2.5 g [16], 5 g [52], 10 g [51], 15 g [17], and 20 g [33] of soil sample have been developed for pesticide-residue analysis, although most authors opted for 5 or 10 g. In all cases, the amount of sample used can be considered relatively low, which in turn is one of the great inherent benefits of the QuEChERS method. However, it must be considered that the extraction is normally carried out in 50-milliliter centrifuge tubes.…”

“…However, other combinations of the same salts, or even different salts, have been assayed to promote ACN/water-phase separation during extraction. In this sense, the combination of anhydrous MgSO 4 and NaCl in 1:1 [39] or 2:1 [32,34,52,53,57] ratios (w/w) have also been used as alternatives to the original ratio, and both salts have even been successfully used alone. As an example, García Pinto et al [16] performed a series of experiments with different combinations of anhydrous MgSO 4 with and without NaCl for the extraction of chloroform, 1,2-dichlorobenzene, and hexachlorobenzene (HCB).…”

“…Consequently, dSPE is a shorter, simpler and more environmentally friendly procedure than conventional SPE. As in the most popular versions, anhydrous MgSO 4 and PSA have been effectively used during pesticide analysis in soil samples [14,17,19,22,53,54,56]. For example, Słowik-Borowiec et al [54] recently used 180 mg of MgSO 4 and 30 mg of PSA per mL of extract for the determination of 94 multiclass pesticides and 13 polycyclic aromatic hydrocarbons in soil samples.…”