Proposal of an international harmonized analytical technique for quantifying of residual acetamiprid and imidacloprid in wheat
Keywords:International Harmonized Analytical Method, Acetamiprid, Imidacloprid, Centrifugal Monolithic Silica Spin Mini-Column.
This paper proposes an international harmonized analytical method for residual monitoring of selected neonicotinoids in crops and presents a fast, easy, and space-saving technique of sample preparation followed by a 100% water mobile phase high-performance liquid chromatography (HPLC) coupled photo-diode array detector (PDA) for quantifying acetamiprid (ATP) and imidacloprid (ICP) in wheat. The analytes were extracted from the sample using a handheld ultrasonic homogenizer with water, and purified by MonoSpin® C18-CX, a centrifugal monolithic silica spin mini-column, and quantified within 20 min/sample. The accuracy, precision, and system suitability are well within the international method acceptance criteria.
 Cressey D (2013) "Europe debates risk to bees", Nature 496, 408. http://dx.doi.org/10.1038/496408a.
 European Commission, Regulation (EU) No 485/2013, 2013. http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2013:139:0012:0026:EN:PDF .
 European Commission, Bees & Pesticides: Commission goes ahead with plan to better protect bees. 30 May 2013. http://ec.europa.eu/food/archive/animal/liveanimals/bees/neonicotinoids_en.htm .
 European Food Safety Authority (EFSA), EFSA assesses po-tential link between two neonicotinoids and developmental neurotoxicity. Press release 17 December 2013. http://www.efsa.europa.eu/en/press/news/131217.htm .
 FAO, FAOSTAT, Retrieved 23 November 2013. http://faostat3.fao.org/browse/Q/*/E .
 Codex Alimentarius, Pesticide Residues in Food and Feed, Codex Pesticides Residues in Food Online Database 2013.
 Chen M, et al (2013) Simultaneous determination of residues in pollen and high-fructose corn syrup from eight neonicotinoid insecticides by liquid chromatography-tandem mass spectrometry. Anal. Bioanal. Chem. 405, 9251-9264. http://dx.doi.org/10.1007/s00216-013-7338-7.
 Xiao Z, et al. (2013) Determination of neonicotinoid insecticides residues in eels using subcritical water extraction and ultra-performance liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta 777, 32-40. http://dx.doi.org/10.1016/j.aca.2013.03.026.
 Jovanov P, et al. (2013) Multi-residue method for determination of selected neonicotinoid insecticides in honey using optimized dispersive liquid-liquid microextraction combined with liquid chromatography-tandem mass spectrometry. Talanta 111, 125-133. http://dx.doi.org/10.1016/j.talanta.2013.02.059.
 Xie W, et al. (2011) Determination of neonicotinoid pesticides residues in agricultural samples by solid-phase extraction combined with liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 1218, 4426-4433. http://dx.doi.org/10.1016/j.chroma.2011.05.026.
 Seccia S, et al. (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, 115-120. http://dx.doi.org/10.1016/j.chroma.2008.10.088.
 Di Muccio A, et al. (2006) Application of solid-phase extraction and liquid chromatography-mass spectrometry to the determination of neonicotinoid pesticide residues in fruit and vegetables. J. Chromatogr. An 1108, 1-6. http://dx.doi.org/10.1016/j.chroma.2005.12.111.
 Ferrer I, et al. (2005) Quantitation and accurate mass analysis of pesticides in vegetables by LC/TOF-MS. Anal. Chem. 77, 2818-2825. http://dx.doi.org/10.1021/ac048458x.
 EU classification (The Dangerous Substances Directive 67/548/EEC): Council Directive 67/548/EEC of 27 June 1967 on the approximation of laws, regulations and administrative provisions relating to the classification, packaging and labelling of dangerous substances.
 Anastas, PT, and Warner, JC, Green Chemistry: Theory and Practice; Oxford University Press: Oxford, United Kingdom (1998).
 Yoshimura, T, et al., Green Chemistry: Aim for the Zero Emission-Chemicals, Sankyo Publishing Co. Ltd. Press, Tokyo, Japan (2001).
 FDA/CDER/CVM, Guidelines for Industry â€“ Bioanalytical Method Validation, 2001. http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/UCM070107.pdf .
 FDA, Reviewer Guide, Validation of Chromatographic Method Center Drug Evaluation and Research (CFDER), Silver Spring, MD, USA, 1994.
 Huber, L, Validation and Quantification in Analytical Laboratories, Interpharm Press, East England, CO, USA, 1998.
 ICH, Work Products, ICH Guidelines, Quality Guidelines- Validation of analytical procedures: Test and methodology Q2 (R1), 1994. http://www.ich.org/products/guidelines.html .
 AOAC International, Guidelines for Standard Method Performance Requirements, 2012. http://www.eoma.aoac.org/app_f.pdf .
 Codex alimentarius commission, ALINORM 01/23, Codex Committee on Methods of Analysis and Sampling, Joint FAO/WHO Food Standards Programme, the 23nd Session of the Codex Committee on Method of Analysis and Sampling, March 2001.
 GL Sciences, Monolithic SPE Column for the Purification and Enrichment of Small Amount Sample, MonoSpinÂ® Series. http://www.glsciences.com/c-product/sample/solid/monospin-series/ .