Application of solid-phase extraction and liquid chromatography-mass spectrometry to the determination of neonicotinoid pesticide residues in fruit and vegetables.

A rapid and simple method for simultaneous analysis of four neonicotinoid insecticides including acetamiprid, imidacloprid, thiacloprid and thiamethoxam in fruit and vegetable matrices has been developed. For instance, ready-to-use cartridges filled with a macroporous diatomaceous material were used to extract in a single step insecticide residues with dichloromethane from aqueous-acetone extracts of fruits and vegetables. The eluate was evaporated, the residue redissolved with methanol and then analyzed by liquid chromatography-mass spectrometry in the electrospray ionization (ESI) positive mode. Average recoveries of the four pesticides were between 74.5 and 105% at both spiking levels 0.1 and 1.0 mg kg(-1) in peach, pear, courgette, celery and apricot. Relative standard deviations (RSDs) were less than 10% for all of the recovery tests. The calculated limits of quantitation (LOQs) (0.1-0.5 mg kg(-1)) were equal or lower then the maximum residue limits (MRLs) established by European legislation (0.1-0.5 mg kg(-1)). The proposed method is fast, easy to perform and could be utilized for monitoring of pesticides residues.

Organochlorine compounds in tissues of swordfish (Xiphias gladius) from Mediterranean Sea and Azores islands.

Polychlorobiphenyls (PCB) and organochlorine (OC) pesticides are endocrine-disrupting chemicals (EDCs). The Italian Ministry of Environment has undertaken a program (1999-2001) to measure levels of contaminants in top marine predators and to develop sensitive biomarkers for the evaluation of toxicological risk in these species. In 1999, 15 swordfishes (Xiphias gladius) taken from the Mediterranean Sea along the Sicilian coast (Strait of Messina, Italy) and in the Atlantic Ocean along the Azores Islands, and analysed for 34 congeners of PCBs and 27 organochlorine (OC) pesticides in gonad, muscle, liver and blubber tissues. In the tissues of Mediterranean swordfishes the sum of the determined PCBs congeners ranged from 4.61 to 4651.17 ng g(-1) on fresh tissue basis. Among organochlorine pesticides DDE, DDT and DDD (TDE) predominated with an overall range of 2.37-4734.56 ng(-1) w.w. In particular p,p'-DDE had concentrations appearing up to 3900 ng(-1), with the highest values found in fatty tissues, such as blubber. In the liver of Azores Island swordfishes lower levels of summation PCBs (8.43-294.17 ng/g w.w.) and summation DDTs (<0.01-217.44 ng/g w.w.) were determined.