Application of QuEChERS method and gas chromatography-mass spectrometry for the analysis of cypermethrin residue in milk

Analytical methods for the isolation and determination of cypermethrin in milk, based on the solid-phase microextraction (SPME) and QuEChERS methods (Quick, Easy, Cheap, Effective, Rugged, and Safe) are presented. The SPME technique was not appropriate to analyse cypermethrin in milk, even establishing the best extraction conditions, polydimethylsiloxane fiber, 60 min time extraction, 60 °C temperature extraction, addition of salt (NaCl) and stirring rate. The extraction efficiency was low probably because of the matrix constituents. The QuEChERS method involves the extraction of the analyte with acetonitrile and simultaneous liquid-liquid partitioning formed by adding anhydrous MgSO(4) plus NaCl, followed by the removal of residual water and cleanup using a procedure called dispersive solid-phase extraction, in which anhydrous MgSO(4) plus PSA and C18 are mixed with 1 mL of acetonitrile extract. The detection and quantification limits were 0.01 and 0.04 mg kg(-1), respectively, and the percentage recovery obtained ranged from 92 to 105% with relative standard deviations below 7%.     

Validation of an analytical method for the quantification of pyrethrins on lemons and apricots using high-performance liquid chromatography/mass spectrometry

An analytical procedure has been developed for the determination of natural pyrethrins (pyrethrin I, pyrethrin II, jasmolin I, jasmolin II, cinerin I and cinerin II) in lemon and apricot. The QuEChERS method, which stands for quick, easy, cheap, effective, rugged and safe was used for extraction. Analysis of the extract was performed by liquid-chromatography-electrospray ionisation-tandem mass spectrometry. The ions prominent in the ESI spectra were [M+H]+ for the six compounds. A Zorbax SB-C18 column was used with a programmed gradient mobile phase consisting of (A) water containing 0.1% formic acid and 5 mM ammonium formate and (B) ACN. The method was linear within the investigated concentration range, displaying a calibration curve correlation factor of 0.99. The coefficients of variation obtained (RSD) were below 20% and the recoveries were in the 70-110% range.     

Determination of sixteen pesticides in peppers using high-performance liquid chromatography/mass spectrometry

A method for the detection and quantification of 16 pesticides: flufenoxuron, fenoxycarb, dimethomorph, acetamiprid, imidacloprid, lufenuron, thiacloprid, thiabendazole, thiophanate-methyl, spinosad, fenbutatin oxide, methoxyfenozide, oxamyl, clothianidin, thiamethoxam and carbendazim has been developed based on high-performance liquid chromatography-mass spectrometry. Pesticide residues were extracted from the samples according to the QuEChERS method which stands for quick, essay, cheap, effective, rugged and safe. Homogenised analytical portions (10 g ± 0.1) of samples of peppers were spiked at two levels (10 and 100 μg kg?1) with a small volume of an appropriate standard mixture solution containing each pesticide. Analyses were performed using electrospray ionization (ESI) and a MSD trap system. Chromatography separation was achieved using a ZORBAX SB-C18 3.5 μm particle size analytical column, 2.1 × 50 mm from Agilent, with gradient elution at a flow-rate of 0.4 mL/min with mobile phases: waters-0.1 % HCOOH-5 mM HCOONH? and MeOH-5 mM HCOONH?. The method has been validated based on the SANCO European Guidelines. Under the optimized conditions the recoveries (n = 7) were in the range 70-110 % with satisfactory precision (CV ≤ 20 %). A linear dynamic range was obtained over a range of concentrations from 10 to 100 μg kg?1 for each of the analytes, with correlation coefficients >0.997.     

Field sampling of soil pore water to evaluate trace element mobility and associated environmental risk

Monitoring soil pollution is a key aspect in sustainable management of contaminated land but there is often debate over what should be monitored to assess ecological risk. Soil pore water, containing the most labile pollutant fraction in soils, can be easily collected in situ offering a routine way to monitor this risk. We present a compilation of data on concentration of trace elements (As, Cd, Cu, Pb, and Zn) in soil pore water collected in field conditions from a range of polluted and non-polluted soils in Spain and the UK during single and repeated monitoring, and propose a simple eco-toxicity test using this media. Sufficient pore water could be extracted for analysis both under semi-arid and temperate conditions, and eco-toxicity comparisons could be effectively made between polluted and non-polluted soils. We propose that in-situ pore water extraction could enhance the realism of risk assessment at some contaminated sites.     

Phytostabilization of semiarid soils residually contaminated with trace elements using by-products: sustainability and risks

We investigated the efficiency of various by-products (sugarbeet lime, biosolid compost and leonardite), based on single or repeated applications to field plots, on the establishment of a vegetation cover compatible with a stabilization strategy on a multi-element (As, Cd, Cu, Pb and Zn) contaminated soil 4-6 years after initial amendment applications. Results indicate that the need for re-treatment is amendment- and element-dependent; in some cases, a single application may reduce trace element concentrations in above-ground biomass and enhance the establishment of a healthy vegetation cover. Amendment performance as evaluated by % cover, biomass and number of colonizing taxa differs; however, changes in plant community composition are not necessarily amendment-specific. Although the translocation of trace elements to the plant biotic compartment is greater in re-vegetated areas, overall loss of trace elements due to soil erosion and plant uptake is usually smaller compared to that in bare soil.     

Impact of soil quality on elemental uptake by, and distribution in, Colocasia esculenta (Amadumbe), an edible root

In this study the elemental distribution of selected essential (Ca, Mg, Al, Mn, Cu, Fe, Co, Cr, Zn, Ni and Se) and the non-essential (Pb, Hg and As) elements were determined in the bulb and peel of Amadumbe (Colocasia esculenta) samples from eight different sites in KwaZulu-Natal, South Africa. The concentration of Se and As in the soil and in the Amadumbe bulbs were below the detection limit of 0.09 μg g?1. The total and bioavailable concentrations of the elements in conjunction with pH, soil organic matter (SOM) and cation exchange capacity (CEC) were determined in the soil samples from the eight sites. Statistical analysis was done to evaluate the impact of soil quality parameters on the chemical composition of the Amadumbe root. The results show accumulation or exclusion of certain elements by the bulb as evidenced by the noticeable increase or decrease of the concentrations of elements, respectively. Ca and Mg were found to be major elements in the range (2000-12000 μg g?1), whilst Mn, Zn, Fe and Al were found to be minor elements in the range (20-400 μg g?1). A general trend observed was that the plant favours the absorption of Zn over Cu. A positive correlation between Mg & Ca, Cu & Fe and Co & Ni was also observed. Statistical analysis revealed that the plant tended to accumulate Mg, Ca, Co, Cr and Pb whilst it excluded Hg and Fe, to a lesser extent.     

Bacterial community composition characterization of a lead-contaminated <Emphasis Type="Italic">Microcoleus</Emphasis> sp. consortium

Introduction  

A Microcoleus sp. consortium, obtained from the Ebro delta microbial mat, was maintained under different conditions including uncontaminated, lead-contaminated, and acidic conditions.     

Phytoremediation of a sulphonated azo dye Green HE4B by <Emphasis Type="Italic">Glandularia pulchella</Emphasis> (Sweet) Tronc. (Moss Verbena)

Purpose  

The dyes and dye stuffs present in effluents released from textile dyeing industries are potentially mutagenic and carcinogenic. Phytoremediation technology can be used for remediating sites contaminated with such textile dyeing effluents. The purpose of the work was to explore the potential of Glandularia pulchella (Sweet) Tronc. to decolorize different textile dyes, textile dyeing effluent, and synthetic mixture of dyes.     

Chitosan membranes as sorbents for trace elements determination in surface waters

Purpose  

Chitosan membranes (non-crosslinked, crosslinked, and modified with l-cysteine) were evaluated as sorbents prior to electrothermal atomic absorption spectrometry (ETAAS) determination of total dissolved metal content in surface water samples.     

Spectrofluorimetric study of the ageing of mixtions used in the gildings of mediaeval wall paintings

Introduction  

In the Middle Ages, we could find gildings on mural paintings. Gold, silver or tin leaves were applied according to distemper or mixtion technique. For the first one, a binder as glue is necessary, and for the second, a lipidic binder is used to stick the metallic leaf. Studies of gildings materials characterization show that the mixtion technique, with a mordant, is the most common. Linseed oil seems to be the binder used. It is always mixed with a siccative agent as lead. Because of bad conditions of conservation, the gildings do not resist anymore, only remain traces of metal or the adhesive under-layer. Thanks to the binder fluorescence, we can nowadays detect ancient gildings.