Application of Hydrophobic Magnetic Nanoparticles as Cleanup Adsorbents for Pesticide Residue Analysis in Fruit, Vegetable, and Various Soil Samples

Abstract

A clean-up procedure based on hydrophobic magnetic nanoparticles for QuEChERS extraction followed by GC-MS method for the simultaneous determination of 16 organochlorine pesticides was developed. The type and amount of clean-up adsorbents (C18/GCB/Fe 3 O 4 /Fe 3 O 4 @Triton), the volume and polarity of the extraction solvent were optimized. The method was validated according to SANTE/11813/2017 and ICH/2005/Q2/R1 guidelines. Spiked-sample recoveries of 84 -108% with RSD below 8% were obtained for all the tested pesticides in strawberry. Quantification was carried out using matrix-matched calibration plots, which displayed good linearity (R 2 > 0.99), the limits of quantification being less than the maximum residue limits (MRL) for food. The elaborated procedure with satisfactory results was applied in to determine the pesticides in fruit, vegetable (strawberries, avocadoes, watermelons, radishes, and flesh kiwis) and soil (agricultural, urban and lab-made) samples. The most frequentlyfounded pesticide residues were: 4,4 4, lindane and 4, cases were below MRL. The highest concentration of 4,4'-DDT was founded in agricultural and lab-made soils.

Design, Preparation, and Application of Magnetic Nanoparticles for Food Safety Analysis: A Review of Recent Advances

“…tested hydrophobic MNPs as an effective cleanup adsorbent for the analysis of 16 pesticides in fruits and vegetables from supermarkets. In their study, magnetic Fe 3 O 4 @Triton adsorbents provided the lowest level of coextracted interference compounds (including organic pigments) in the food samples and showed better cleanup performance than the commercial adsorbent (C18 and GCB) …”

“…In addition, the MNP surface can be modified with polymeric properties, which present broad application prospects in analytical science, food safety monitoring, biomedicine, immunoassay, magnetic resonance imaging, immobilization enzymes, environmental engineering, and proteomics, among many other fields. − Moreover, most MNPs are also environmentally friendly, which often can be recollected and used multiple times to avoid pollution. And a large number of food safety analysis methods, typified by magnetic solid-phase extraction (MSPE), have been developed based on these magic magnetic nanohelpers. , …”

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.…”

“…The original approach, which involves adding anhydrous magnesium sulphate and sodium chloride in the extraction step, has found several applications for the analysis of pesticide residues in soils [18,22,26,28,37,38,48]. Furthermore, many researchers have used extraction liquid-liquid partitioning based on the AOAC Official Method 2007.01, which involves the use of acetic acid (HAc) in can, plus anhydrous MgSO 4 and NaOAc (relatively strong buffering capacity) [31], and the CEN Standard Method EN 15662 approach, which uses ACN followed by anhydrous MgSO 4 and NaCl, as well as sodium citrate tribasic dihydrate and sodium citrate dibasic sesquihydrate as the buffer (with a relatively low buffering capacity) [14,19,20,24,27,30,36,44,51].…”

“…In this relatively novel approach, named magnetic d-SPE, bare magnetite (Fe 3 O 4 ) is the most widely used MNP for a number of applications in pesticide-residue analysis, but its selectivity is relatively poor. In the study by Hubetska et al [48], Fe 3 O 4 @Triton was compared with C 18 , GCB, and Fe 3 O 4 for the determination of 16 OCPs in avocado and strawberry samples. The nonionic surfactant, Triton X-100, was used as a precursor for the synthesis of the functionalized MNPs because it contains several functional complexes that can selectively bind to pesticides.…”