Comparison of four extraction methods for the analysis of 24 pesticides in soil samples with gas chromatography-mass spectrometry and liquid chromatography-ion trap-mass spectrometry.

With a view to analyse multiresidues of pesticides in soil samples, a new ultrasonic solvent extraction (USE) was compared to the European Norm DIN 12393 for foodstuff (extraction with acetone, partitioning with ethylacetate/cyclohexane and clean-up with gel permeation chromatography (GPC)), the QuECheRS method and a pressurised liquid extraction (PLE) method. Pesticides were analysed with both GC-MS and HPLC-MS/MS. The reference materials were the EUROSOIL 7 and its subsoil SO26 as well as a sea sand. All the substances were observed to be linear in the range of 4-800 ng g(-1) for the European Norm DIN 12393, 7-1400 ng g(-1) for the USE method and 20-4000 ng g(-1) for the QueCheRS and the PLE methods. Limits of detection (LOD) and limits of quantification (LOQ) were with HPLC between 0.006 and 0.23 ng g(-1) and between 0.022 and 0.77 ng g(-1), respectively, with the exception of diuron (LOD up to 11.8 ng g(-1); LOQ up to 39.2 ng g(-1)). With GC they ranged from 3.0 to 87.5 ng g(-1) and from 10 to 292 ng g(-1), respectively. All substances could be recovered with USE as well as with the QuECheRS method; the European Norm DIN 12393 could not recover carbendazim and metamitron; the PLE carbendazim, metamitron and monolinuron. For the remaining substances, recoveries at a 500 ng g(-1) fortification level ranged from 10.9 to 96.3% with the USE. In comparison, the QuECheRS method was the most efficient extraction method with recoveries from 27.3 to 120.9%. It was followed by the European Norm DIN 12393 with recoveries between 6.8 and 108.1% and the PLE with recoveries from 12.2 to 153.2%. Recoveries were higher from the EUROSOIL 7 than from the SO 26. The repeatability expressed in term of standard deviation was below 20% for all substances and all materials.

Arsenic contamination of soils and agricultural plants through irrigation water in Nepal.

This study monitored the influence of arsenic-contaminated irrigation water on alkaline soils and arsenic uptake in agricultural plants at field level. The arsenic concentrations in irrigation water ranges from <0.005 to 1.014 mg L(-1) where the arsenic concentrations in the soils were measured from 6.1 to 16.7 mg As kg(-1). The arsenic content in different parts of plants are found in the order of roots>shoots>leaves>edible parts. The mean arsenic content of edible plant material (dry weight) were found in the order of onion leaves (0.55 mg As kg(-1))>onion bulb (0.45 mg As kg(-1))>cauliflower (0.33 mg As kg(-1))>rice (0.18 mg As kg(-1))>brinjal (0.09 mg As kg(-1))>potato (<0.01 mg As kg(-1)).

Pesticide and non-dioxin-like polychlorinated biphenyls (NDL-PCBs) residues in foodstuffs from Ismailia city, Egypt.

Samples of vegetables and cereals from Egypt were screened for 113 pesticides, of which 68 were quantified, using gas chromatography-mass spectrometry (GC/MS) with limits of detection (LODs) ranging from 0.02 to 1.9 µg kg⁻¹. In addition, the residues of 17 non-dioxin-like polychlorinated biphenyls (NDL-PCBs) were measured in samples of animal origin (meat, dairy products and seafood) using high-resolution gas chromatography (HRGC)/high-resolution mass spectroscopy (HRMS). None of the cereal samples and 72.7% of the vegetables contained any detectable levels of the pesticides. Detectable residues, not exceeding the current European Union maximum residue limits (MRLs) were found in 27.3% of vegetables. The estimated daily intake for detected pesticides was well below their corresponding acceptable daily intake (ADI), with exposure ranges between 0.002% of the ADI for profenofos and 0.2% of the ADI for lambda-cyhalothrin. The sum concentration of 17 PCBs congeners varied between 2.5 and 322 ng g⁻¹ fat, corresponding to 1.7-216 ng g⁻¹ fat for the seven indicator PCBs. The highest values were measured in seafood, the lowest in dairy products. Hexa-CB 153, 138 and hepta-CB180 were the congeners with the highest contribution. PCBs congener profiles found in most of the samples were consistent with the expected profile for Aroclor 1260 and 1262. PCBs' contamination levels reported in this paper were many times lower than in developed countries, except for chicken samples. Also, the dietary intake of seven indicator PCBs due to the consumption of food of animal origin (4.84 ng kg⁻¹ body weight day⁻¹) from Ismailia city, Egypt, is several times lower than the intake in European Union countries.

Certification of the European reference soil set (IRMM-443--EUROSOILS). Part I. Adsorption coefficients for atrazine, 2,4-D and lindane.

The European Commission has characterised and certified a set of six European soils (the EUROSOILS) under the number IRMM-443. After a successful validation and trial period with a preliminary batch it was decided to produce a new batch of certified reference materials. Part I of this paper describes the certification of adsorption coefficients for atrazine, 2,4-D and lindane in these soils. The adsorption coefficients were determined according to OECD Test Guideline 106. Additionally, the underlying principles for the value assignment process according to the GUM and their practical application to the numerical data obtained during the certification exercise according to ISO Guide 34 and 35 are discussed.

Certification of the European Reference Soil Set (IRMM-443--EUROSOILS). Part II. Soil-pH in suspensions of water and CaCl2.

IRMM-443 re-groups a set of six European Reference Soils (EUROSOILS), which had been certified for their adsorption coefficients for atrazine, 2,4-D and lindane (Certification of the European Reference Soil Set (IRMM-443-EUROSOILS)-Part I. Adsorption coefficients for atrazine, 2,4-D and lindane. Sci Total Environ, in press). The certification of these parameters was complemented by an additional certification of pH in suspension as well by the determination of indicative values for total nitrogen, organic and total carbon content. While Part I explained the principles of the value assignment process and discussed their application to the adsorption coefficients, Part II presents the certified values for pH as well as the indicative values for N(tot), C(tot) and C(org). In addition, the assessment of uncertainty components for stability and homogeneity, which have been included in the final uncertainty budget, is discussed.