A modified QuEChERS and LC–MS/MS method has been developed for the simultaneous determination of residues of six neonicotinoids in various crops, including spinach, cucumber, apple and pomelo. The method showed good linearity (R2 ≥ 0.9995) and precision (RSD ≤ 14.0%). Average recoveries of the six neonicotinoids ranged between 73.7% and 103.8% at spiking levels 0.005, 0.1 and 1 mg kg−1. The LODs and LOQs were in the ranges of 0.20–0.85 μg kg−1 and 0.66–2.84 μg kg−1, respectively. The method was satisfactorily validated for the analysis of 50 agricultural samples. Imidacloprid and imidaclothiz were detected at concentration levels ranging from 7 to 5.3 μg kg−1.
Neonicotinoid Insecticide QuEChERS LC–MS/MS
The authors are grateful for the support from Chinese National Modern Industrial Technology System Foundation, P. R. of China (Project No: CARS-09-G15) and Chinese National Natural Science Foundation Support (Project No: 31171872).
Costel S, Rodica DN, Agata KW, Shela G, Andrzej W, Jacek N (2012) Classification and fingerprinting of kiwi and pomelo fruits by multivariate analysis of chromatographic and spectroscopic data. Food Chem 130:994–1002CrossRefGoogle Scholar
Ferrer I, Thurman EM, Fernandez-Alba AR (2005) Quantitation and accurate mass analysis of pesticides in vegetables by LC/TOF-MS. Anal Chem 77:2818–2825CrossRefGoogle Scholar
Fidente P, Seccia S, Vanni F, Morrica P (2005) Analysis of nicotinoid insecticides residues in honey by solid matrix partition clean-up and liquid chromatography–electrospray mass spectrometry. J Chromatogr A 1094:175–178CrossRefGoogle Scholar
Liu S, Zheng Z, Wei F, Ren Y, Gui W, Wu H, Zhu G (2010) Simultaneous determination of seven neonicotinoid pesticide residues in food by ultraperformance liquid chromatography tandem mass spectrometry. J Agric Food Chem 58:3271–3278CrossRefGoogle Scholar
Muccio AD, Fidente P, Attard Barbini D, Dommarco R, Seccia S, Morrica P (2006) Application of solid-phase extraction and liquid chromatography–mass spectrometry to the determination of neonicotinoid pesticide residues in fruit and vegetables. J Chromatogr A 1108:1–6CrossRefGoogle Scholar
Nauen R, Ebbinghaus-Kintscher U, Schmuck R (2001) Uptake, translocation and metabolism of imidacloprid in plants. Pest Manag Sci 57:577–586CrossRefGoogle Scholar
Seccia S, Fidente P, Montesano D, Morrica P (2008) Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection. J Chromatogr A 1214:115–120CrossRefGoogle Scholar
Shashi BS, Foster GD, Khan SU (2004) Microwave-assisted extraction for the simultaneous determination of thiamethoxam, imidacloprid, and carbendazim residues in fresh and cooked vegetable samples. J Agric Food Chem 52:105–109CrossRefGoogle Scholar
Watanabe E, Baba K, Eun H (2007) Simultaneous determination of neonicotinoid insecticides in agricultural samples by solid-phase extraction cleanup and liquid chromatography equipped with diode-array detection. J Agric Food Chem 55:3798–3804CrossRefGoogle Scholar
Wu M, Cai J, Yao J, Dai B, Lu Y (2010) Study of imidaclothiz residues in cabbage and soil by HPLC with UV detection. Bull Environ Contam Toxicol 84:289–293CrossRefGoogle Scholar
Xiao Z, Li X, Wang X, Shen J, Ding S (2011) Determination of neonicotinoid insecticides residues in bovine tissues by pressurized solvent extraction and liquid chromatography–tandem mass spectrometry. J Chromatogr B 879:117–122CrossRefGoogle Scholar
Zofia L, Waldemar K, Piotr G, Lidia S (2010) Amino acid profile of raw and as-eaten products of spinach (Spinacia oleracea L.). Food Chem 126:460–465Google Scholar