Modified QuEChERS Method for Extracting Thiamethoxam and Imidacloprid from Stingless Bees: Development, Application, and Green Metrics

Abstract

In the present study, a method for the determination of residues of the neonicotinoid insecticides thiamethoxam and imidacloprid in the stingless bee Melipona scutellaris Latreille (1811) was optimized through a factorial design, tested using green metrics, and then applied to exposed bees. It combines the extraction with a modified quick, easy, cheap, effective, rugged, and safe method and the determination by liquid chromatography–tandem mass spectrometry analysis. Different parameters such as the mass of the sample, dispersive sorbents, and elution solvents were assessed. Method validation parameters were checked and include sensitivity, specificity, and linearity. The limit of quantification of 0.0025 μg g–1 was obtained for both insecticides, where accuracy was 94%–100% with satisfactory intraday and interday precisions (relative standard deviation <10%). The qualified method was applied to orally and topically exposed bee samples, and the results indicated that it is suitable for the determination and quantification of neonicotinoid pesticide residues in this species. Moreover, green analytical metrics like the National Environmental Methods Index, Eco Scale score, high‐performance liquid chromatography with an environmental assessment tool (HPLC‐EAT), waste generation, and amount of sample were compared with methods described in the literature involving neonicotinoid analysis in honeybees. As a result, the present study displayed the highest Eco Scale score and HPLC‐EAT score and the second smallest amount of sample and waste generated. Thus, the method meets green analytical metrics more than other methods. In this sense, besides the application, the multicriteria decision analysis tool employed suggests that this is a good option as a green analytical method. Environ Toxicol Chem 2022;41:2365–2374. © 2022 SETAC

Contact exposure of honey bees and social stingless bees to fungicide sprayed on cotton and soybean in a controlled field simulation system

“…After validation of the tests for determining the retention times of the a. i., the bee samples were dried in a freeze dryer LioBras, model Liotop K107, for a period of 24 hours. After drying, the samples were submitted to extraction and clean-up processes using a modification of the QuEChERS method (Rahman et al, 2022): 5 mL of acetonitrile was added and 0.4 g of MgSO 4 , 0.1 g of NaCl, 0.1 g of sodium citrate tribasic dihydrate (SCTD) and 0.05 g of sodium citrate dibasic sesquihydrate (SCDS) were used for the extraction of a sample containing 20 honey bees. For clean-up, 37.7 mg of MgSO 4 , 6.3 mg of primary secondary amine (PSA) and 6.3 mg of C18 were employed.…”

Characterization of the Metabolites of Neonicotinoid Insecticide Imidaclothiz in Mice

“…Therefore, sample pretreatment methods and analytical instruments play a vital role in the precise analysis of metabolites. Quick, easy, cheap, effective, rugged, and safe extraction (QuEChERS) is a conventional extraction and purification technique that ensures the accurate routine analysis of neonicotinoid compounds in various matrices. − Ultrahigh-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) has been increasingly utilized to explore chemical degradation pathways and identify metabolites. Its high resolution and efficient tandem mass spectrometry are the essential analytical capabilities for the in-depth analysis of extremely complex mixtures of (bio)molecules of a very broad and dynamic range of concentrations .…”