Determination of Acetamiprid, Imidacloprid, and Nitenpyram Residues in Vegetables and Fruits by High-Performance Liquid Chromatography with Diode-Array Detection

Abstract

Determination of 3 neonicotinoid insecticides, nitenpyram, imidacloprid, and acetamiprid, was studied. Vegetables and fruits were extracted with acetonitrile. The crude extract was passed through a weak anion-exchange cartridge (PSA). The effluent was subjected to silica gel cartridge. Imidacloprid and acetamiprid were eluted with 10 mL of 4:6 (v/v) acetone/hexane, followed by nitenpyram with acetone (20 mL). Pesticides were determined by HPLC with a C-18 column and diode-array detection system. Imidacloprid and acetamiprid were recovered at about 90% at the spike levels with 0.2 and 2 mg/kg in cucumber, potato, tomato, eggplant, Japanese radish, and grape. Nitenpyram was recovered at 64-80%. Relative standard deviations were less than 10% throughout all the recovery tests. In the residue analysis, agriculturally incurred pesticides at 0.08-0.14 mg/kg were designated with UV spectra compared with respective reference standards.

Two fatal intoxication cases with imidacloprid: LC/MS analysis

“…Several methods have been published for the determination by high-performance liquid chromatography of imidacloprid and its main metabolites in soils [11][12][13], in fruits and vegetables [14][15][16][17][18][19][20][21], in water [13] and even in air [22,23]. No methods have been published for the determination of this insecticide in human samples.…”

Dissipation rate of acetamiprid in sweet cherries

“…Imidacloprid was extracted with acetone and transferred to a mixture of dichloromethane and petroleum ether to reduce interferences (Fernandez-Alba et al, 1996). The use of dichloromethane in these methods is not advisable because of environmental concerns (Obana et al, 2002).…”

Review on Current Analytical Methods with Chromatographic and Nonchromatographic Techniques for New Generation Insecticide Neonicotinoids

“…Table 1 shows that sample pre-treatment procedures roughly consist of (1) extraction of the target pesticide from the sample and (2) separation of the target pesticide from the extract and clean-up. For (1) extraction of neonicotinoid insecticides, shaking extraction with organic solvents such as acetone, acetonitrile, or methanol (Baskaran et al, 1997;de Erenchun et al, 1997;Mohan et al, 2010;Tokieda et al, 1997bTokieda et al, , 1998, blending extraction with a homogenizer (Agüera et al, 2004;Blasco et al, 2002aBlasco et al, , 2002bDi Muccio et al, 2006;Fernandez-Alba et al, 1996Ferrer et al, 2005;Hengel & Miller, 2008;Hernández et al, 2006;Ishii et al, 1994;Jansson et al, 2004;Kamel et al, 2010;Mateu-Sánchez et al, 2003;Obana et al, 2002Obana et al, , 2003Sannino et al, 2004;Ting et al, 2004;Tokieda et al, 1997aTokieda et al, , 1997bVenkateswarlu et al, 2007), and ultrasonic extraction (Bourgin et al, 2009;García et al, 2007;Ishii et al, 1994;Liu et al, 2005Liu et al, , 2010Mayer-Helm, 2009;Rancan et al, 2006aRancan et al, , 2006bZhang et al, 2010) are commonly used. In addition to these, Bourgin et al (2009) extracted five insecticides including imidacloprid from seeds coated with acetonitrile and Xiao et al (2011) extracted seven neonicotinoid insecticides from bovine tissues with water by accelerated solvent extraction (ASE) to give quantitative extraction efficiency.…”

“…a large amount of organic solvent is used; and an emulsion is formed at the liquid-liquid interface depending on the extraction sample that is used. For that reason, it has been increasingly replaced by clean-up mainly by SPE (Mohan et al, 2010;Obana et al, 2002;Ting et al, 2004;. used re-extraction with diatomaceous earth SPE and clean-up with GCB/NH 2 SPE in the development of simultaneous analysis by HPLC-DAD of seven neonicotinoid insecticides released on the market.…”