Dietary exposure to pesticide residues and associated health risks in infants and young children - Results of the French infant total diet study.

A total diet study (TDS) was undertaken to estimate the chronic dietary exposure to pesticide residues and health risks for the French infants and young children below 3 years old. As a whole, 516 pesticides and metabolites were analysed in 309 food composite samples including 219 manufactured baby foods and 90 common foods, which cover 97% of infants and young children's diet. These composite samples were prepared using 5,484 food products purchased during all seasons from 2011 to 2012 and processed as consumed.

Development and Validation of Ion Chromatography-Tandem Mass Spectrometry-Based Method for the Multiresidue Determination of Polar Ionic Pesticides in Food.

An extraction method using acidified methanol based on the quick polar pesticide (QuPPe) method using suppressed ion chromatography coupled to mass spectrometry was developed and validated for the direct analysis of polar pesticides, without the need for derivatization or ion pairing, in cereals and grapes. The method was robust, and results for glyphosate, aminomethyl phosphonic acid (AMPA), N-acetyl-AMPA, glufosinate, 3-methylphosphinicopropionic acid (3-MPPA), N-acetyl glufosinate, ethephon, chlorate, perchlorate, fosetyl aluminum, and phosphonic acid at three concentration levels (typically 0.01, 0.

Identification in residue analysis based on liquid chromatography with tandem mass spectrometry: Experimental evidence to update performance criteria.

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is one of the most widely used techniques for identification (and quantification) of residues and contaminants across a number of different chemical domains. Although the same analytical technique is used, the parameters and criteria for identification vary depending on where in the world the analysis is performed and for what purpose (e.g.

A microelectromechanical systems-enabled, miniature triple quadrupole mass spectrometer.

Miniaturized mass spectrometers are becoming increasingly capable, enabling the development of many novel field and laboratory applications. However, to date, triple quadrupole tandem mass spectrometers, the workhorses of quantitative analysis, have not been significantly reduced in size. Here, the basis of a field-deployable triple quadrupole is described.

Testing a cumulative and aggregate exposure model using biomonitoring studies and dietary records for Italian vineyard spray operators.

The need for improved tools to estimate the cumulative and aggregate exposure to compounds such as plant protection products (PPPs) is recognised in the EU Regulation 1107/2009. A new model has been developed to estimate the exposure within a population to single compounds or compounds within a Cumulative Action Group, considering dietary and non-dietary sources and multiple exposure routes. To test the model a field study was carried out in Italy with operators applying tebuconazole fungicides, with measurements of dermal exposure collected.

Evaluation and validation of an accurate mass screening method for the analysis of pesticides in fruits and vegetables using liquid chromatography-quadrupole-time of flight-mass spectrometry with automated detection.

This study reports the development and validation of a screening method for the detection of pesticides in 11 different fruit and vegetable commodities. The method was based on ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-QTOF-MS). The objective was to validate the method in accordance with the SANCO guidance document (12571/2013) on analytical quality control and validation procedures for pesticide residues analysis in food and feed.

Investigation into the occurrence in food of veterinary medicines, pharmaceuticals, and chemicals used in personal care products.

Human exposure to emerging contaminants by indirect routes is of increasing interest. This study assessed the contamination of food by chemicals used in human pharmaceuticals (HPs), veterinary medicines (VMs), and personal care products (PCPs). A prioritization study was undertaken to identify the chemicals and food-producing scenarios most likely to result in contamination of food.

Can the unauthorised use of ceftiofur be detected in poultry?

Ceftiofur is a third-generation cephalosporin antibiotic used to treat cattle and swine for bacterial infection of the respiratory tract. It is not authorised for use in poultry within the European Union. Due to the complexity of the chemistry and metabolism of ceftiofur, maximum residue limits (MRLs) are based on desfuroylceftiofur (DFC) equivalents after chemical conversion of all compounds that have an intact ß-lactam ring.

Investigation of the fate of trifluralin in shrimp.

Juvenile Pacific white shrimp (Litopenaeus vannamei) were exposed to trifluralin at 0.1 and 0.01 mg L(-1) for 72 h under controlled conditions.

Development and independent laboratory validation of a simple method for the determination of paraquat and diquat in potato, cereals and pulses.

A new sensitive, fast and robust method for the determination of paraquat and diquat residues in potatoes, cereals and pulses is presented. Different extraction conditions (solvent, time and temperature) have been evaluated using barley grain, potatoes and dry lentils containing incurred residues of diquat and paraquat. The finalised procedure involves extraction with a mixture of methanol/water/hydrochloric acid at 80 °C and analysis by liquid chromatography-tandem mass spectrometry.

Investigation into the experimental protocols required to determine maximum residue limits (MRLs) in honey.

There is current debate within the EU, and internationally, on how withdrawal periods and maximum residue limits (MRLs) may be set for honey production. Whilst comprehensive EU guidelines exist for calculating the withdrawal times of veterinary medicines in most food-producing species, the analytical variables to be studied for bees/honey are not well defined. The objective of this study was therefore to investigate and understand the factors, for example sampling variability, that is important in the development of a harmonized protocol that can be used to generate the robust scientific data necessary to assist risk assessors in proposing MRLs for honey.

Uptake and depuration of pharmaceuticals in aquatic invertebrates.

The uptake and depuration of a range of pharmaceuticals in the freshwater shrimp (Gammarus pulex) and the water boatman (Notonecta glauca) was studied. For one compound, studies were also done using the freshwater snail Planobarius corneus. In G.

Study of the depletion of lincomycin residues in honey extracted from treated honeybee (Apis mellifera L.) colonies and the effect of the shook swarm procedure.

Bee colonies were treated with 1.2g lincomycin hydrochloride per hive (single treatment in sucrose solution) and samples of honey were then collected at intervals over a 41-week period. The samples were analysed for lincomycin using Liquid Chromatography-Mass Spectrometry/Mass Spectrometry (LC-MS/MS).

Quantification and screening of pesticide residues in food by gas chromatography-exact mass time-of-flight mass spectrometry.

A gas chromatography-exact mass time-of-flight mass spectrometry (GC-TOF-MS) method has been developed for the quantification of approximately one hundred pesticides in baby food, pear and lettuce samples. Prior to analysis, co-extractives were removed from acetonitrile:toluene (80:20) extracts using dispersive solid-phase extraction with primary secondary amine (50mg) and carbon sorbent (50mg). The concentration of pesticides in the extracts was measured using an extracted mass chromatogram window of 0.

Development and validation of an analytical method for total amitraz in fruit and honey with quantification by gas chromatography-mass spectrometry.

The EU maximum residue limit (MRL) definition for amitraz is 'the sum of amitraz plus all its metabolites containing the 2,4-aniline moiety, expressed as amitraz'. A rapid and sensitive method has been developed and validated in-house for the determination of total amitraz in pears, strawberries, oranges and honey. Samples were hydrolysed (under acidic followed by alkaline conditions) to convert amitraz to 2,4-dimethyaniline, which was then partitioned into 2,2,4-trimethylpentane prior to quantification by gas chromatography-mass spectrometry.

Ultra-performance liquid chromatography for the determination of pesticide residues in foods by tandem quadrupole mass spectrometry with polarity switching.

An ultra-performance liquid chromatographic (UPLC) electrospray ionisation tandem quadrupole mass spectrometric method has been developed for the determination of 52 pesticides in cereal-based baby foods, oranges and potatoes. The fast polarity switching capability of the mass spectrometer used enabled the determination of 44 of the compounds in the positive ionisation mode and 8 of the compounds in the negative ionisation mode in a single run. Prior to analysis, co-extractives were removed from acetonitrile extracts using dispersive solid-phase extraction with primary secondary amine (50 mg).

Measurement uncertainty associated with sample processing of oranges and tomatoes for pesticide residue analysis.

The homogeneity of analytical samples and the stability of pesticides during the sample processing of oranges and tomatoes were evaluated. The mean concentrations of 14C-labeled chlorpyrifos in analytical portions (subsamples) after processing show that homogeneity is dependent on sample type as well as the processing procedure. The homogeneity of analytical samples of tomatoes processed cryogenically was much better than those processed at ambient temperature.

Application of programmable temperature vaporisation injection with resistive heating-gas chromatography flame photometric detection for the determination of organophosphorus pesticides.

The combination of a programmable temperature vaporisation (PTV) injector with resistive heating GC (RH-GC), a form of fast GC, has been applied to the analysis of organophosphorus (OP) pesticides. The PTV injector was optimised in the 'at-once' solvent vent mode for the injection of ethyl acetate (10-40 microL) or ACN (10 microL). The short RH-GC column (5 m x 0.

Semiautomated determination of pesticides in water using solid phase extraction disks and gas chromatography-mass spectrometry.

A method based on semiautomated solid phase extraction using octadecyl-bonded silica disks and gas chromatography-mass spectrometry, operated in selected ion monitoring mode, allows detection and quantification of approximately 100 pesticides and transformation products in drinking water. Samples (500 mL) were passed through the disk, and the retained pesticides were eluted with acetone and ethyl acetate. Typical recoveries for pesticides at 0.

Comparison of ultra-performance liquid chromatography and high-performance liquid chromatography for the determination of priority pesticides in baby foods by tandem quadrupole mass spectrometry.

Determination of 16 priority pesticides and transformation products specified in the EU Baby Food Directive 2003/13/EC has been compared using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) coupled to tandem quadrupole mass spectrometry (MS/MS). Prior to analysis, co-extractives were removed from acetonitrile extracts using dispersive solid-phase extraction (SPE) with primary secondary amine (50 mg). Extracts spiked with pesticides at 1 microg kg(-1) yielded average recoveries in the range 85-119%, with relative standard deviations less than 17%.

Determination of priority pesticides in baby foods by gas chromatography tandem quadrupole mass spectrometry.

A gas chromatography-tandem quadrupole mass spectrometry (GC-MS/MS) method for the determination of twelve priority pesticides, and transformation products (e.g. metabolites) specified in the EU Baby Food Directive 2003/13/EC is described.

Evaluation of gas chromatography-tandem quadrupole mass spectrometry for the determination of organochlorine pesticides in fats and oils.

A gas chromatography-tandem quadrupole mass spectrometry multi-residue method for the analysis of 19 organochlorine pesticides in fats and oils has been developed. Gel permeation chromatography was employed to remove lipid material prior to GC-MS/MS analysis. Average recoveries of the pesticides spiked at 10 and 50 microg kg(-1) into fish oil, pork fat, olive oil and hydrogenated vegetable oil were typically in the range 70-110% with relative standard deviations generally less than 10%.

Method validation of resistive heating--gas chromatography with flame photometric detection for the rapid screening of organophosphorus pesticides in fruit and vegetables.

A rapid method for the screening of organophosphorus (OP) pesticides in fruit and vegetables is reported. Sample extracts were analysed using resistive heating-gas chromatography (RH-GC) with flame photometric detection (FPD). A CarboFrit insert in the GC liner allowed injection of crude extracts onto the GC system.

A multi-residue screening method for the determination of 73 pesticides and metabolites in fruit and vegetables using high-performance liquid chromatography/tandem mass spectrometry.

A multi-residue screening method was developed for the simultaneous analysis of 73 pesticides and their metabolites using high-performance liquid chromatography coupled with electrospray tandem mass spectrometry. These pesticides were determined under a single set of experimental conditions involving a simple acetonitrile extraction without the requirement for a clean-up step. Validation was achieved at 0.