DNA Damage and Effects on Antioxidative Enzymes in Earthworm (Eisenia fetida) Induced by Flumorph

Flumorph is an Oomycete fungicide, which is used extensively as an effective fungicide in vegetables and fruits, but little is known about its effect on nontarget soil organisms. In the present study, biochemical responses including changes in the activity of antioxidative enzymes catalase (CAT), superoxide dismutase (SOD), glutathione-S-transferase (GST), malondialdehyde (MDA), and DNA damage induced by flumorph were investigated in earthworms (Eisenis fetida). The CAT concentrations were stimulated at 5.0 mg kg^?1 over 28 days and inhibited at 10 and 20 mg kg^?1, except 10 mg kg^?1 on days 21 and 28 compared with the controls. The overall SOD activities were inhibited except 5 mg kg^?1 on day 28 and 10 mg kg^?1 on days 7 and 14. Meanwhile, the GST activities were stimulated on day 7 and decreased on the other days in summary. The MDA activities were increased notably at 5, 10, and 20 mg kg^?1 after 14 days. Clear dose-dependent DNA damage to Eisenia fetida was observed by olive tail moments in comet assay compared with controls. The results demonstrate that flumorph induces oxidative stress and DNA damage to earthworms, and the effects may be the important mechanisms of its toxicity.     

Analysis of bioaccessible concentration of trace elements in plant based edible materials by INAA and ICPMS methods

The total metal concentration and bioaccessible concentration of Cr, Mn, Fe, Cu, Zn, Se in Momordica charantia, Asparagus racemosus, Terminalia arjuna and Syzyzium cumini were measured by instrumental neutron activation analysis and by inductively coupled plasma mass spectrometry analysis (ICP-MS). The bioaccessible concentrations were determined in the gastrointestinal digest obtained after treating dried powdered samples sequentially in gastric and intestinal fluid of porcine origin at physiological conditions. The bioaccessible concentration of Fe was in the range of 58–67 mg kg^?1, Mn was 10.2–14.6 mg kg^?1, Cu was 3.7–4.8 mg kg^?1 and Zn was 10.6–18.4 mg kg^?1, were within the safety limits set for vegetable food stuff set by Joint FAO/WHO. The bioaccessibility of Zn, an essential element, was high (40–50 %) in M. charantia and in S. cumini. In addition, the total metal contents and bioaccessible concentration of Ni, Se, Cd and Pb in these samples were measured by ICP-MS. The total Cd content in S. cumini (2.6 ± 0.2 mg kg^?1) and its bioaccessible concentration (0.6 mg kg^?1) were strikingly high as compared to the other samples. Though total Hg contents were determined by ICP-MS, but their bioaccessible concentrations were below the detection limit (0.036 mg kg^?1).     

Rare earth element (REE) in surface mangrove sediment by instrumental neutron activation analysis

A study is carried out on the concentrations of rare earth element (REE) elements present in surface mangrove sediments from 10 locations throughout west coast Malaysia. In carrying out the analysis, the best and most convenient method being the instrumental neutron activation analysis (INAA). Samples were obtained, dried, crushed to powdery form and samples prepared for INAA. All the samples for analysis were weighted approximately 150 mg for short irradiation and 200 mg for long irradiation time. As calibration and quality control procedures, blank samples, standard reference material SL-1 were then irradiated with thermal neutron flux of 4 × 10¹² cm^?2 s^?1 at the MINT TRIGA Mark II research reactor which operated at 750 kW by using a pneumatic transport facility. The REE elements of surface sediment samples in this study are Dy, Sm, Eu,Yb, Lu, Tb, La and Ce. It was found that the level of concentrations of all the REE elements varies in the range (0.35–117.4 mg/kg). The geochemical behavior of REEs in surface sediments and normalized pattern (chondrite and shale) has been studied. The degree of sediments contaminations were computed using an enrichment factor. The results showed that the enrichment factor varied in the range (0.75–6.75).     

Uncertainty Analysis of Chlormequat Residue in Fruits by LC�CMS�CMS

A method for determination of chlormequat (CCC) residue in fruits by liquid chromatography?Ctandem mass spectrometry (LC?CMS?CMS) was developed. Residue of CCC was extracted from samples with methanol?Cwater (v/v, 1:1) containing 1.0% acetic acid, cleaned up by strong cationic exchange (SCX) cartridge, and then determined by LC?CMS?CMS. The method showed good linearity over the concentration range 0.002?C5.0 mg kg^?1 with correlation coefficient above 0.997. The limit of detection (LOD) and limit of quantitation (LOQ) for CCC were 5 × 10^?4 mg kg^?1 (S/N = 3) and 0.002 mg kg^?1 (S/N = 10), respectively. Recoveries for CCC at three spiked levels (0.025, 0.050, and 0.20 mg kg^?1) were in the range 80?C102%. Estimation of measurement uncertainty was calculated for CCC at the level of 0.025 mg kg^?1 in fruits. The results demonstrated that the uncertainty of recovery was the main contribution to the combined standard uncertainty. The relative combined standard uncertainties associated with the method ranged from 11 to 13%, depending on the sample matrices.     

International comparison of the determination of the mass fraction of cadmium, chromium, mercury and lead in polypropylene: the Comité Consultatif pour la Quantité de Matière pilot study CCQM-P106

The CCQM-P106 pilot study was organized by the inorganic working group of the Comité Consultatif pour la Quantité de Matière (CCQM) as a feasibility comparison to study the applicability of different analysis methods to the polypropylene sample and test the abilities of the participants for measuring the Cd, Cr, Hg and Pb in polypropylene. National Institute of Metrology P.R. China (NIM) acted as the coordinating laboratory of this pilot study. There were 21 laboratories that submitted the final results. The median values of the mass fraction of Cd, Cr, Hg and Pb were 36.12 mg kg^?1 (the median absolute deviation about the median (MADe) = 0.46 mg kg^?1), 252.5 mg kg^?1 (MADe = 3.4 mg kg^?1), 387.0 mg kg^?1 (MADe = 10.1 mg kg^?1) and 466.2 mg kg^?1 (MADe = 8.9 mg kg^?1), respectively. Isotope dilution mass spectrometry (IDMS), inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), instrumental neutron activation analysis (INAA) and X-ray fluorescence (XRF) measurement methods were used, and microwave digestion was used by the most of the participants. In general, very good agreement of the results was observed. Moreover, compared to the results of other methods, the results of IDMS still showed less spread amongst laboratories and had a smaller uncertainty. In addition, the results of some analytes used by XRF and INAA also got satisfactory agreement with the median value.     

Analysis of trans-Resveratrol in Iranian Grape Cultivars by LC

In this study, trans-resveratrol levels were determined in 147 Iranian grape cultivars using a modified extraction and gradient HPLC procedure with photodiode array detection. It was found that 41 out of 147 cultivars contained significant levels of trans-resveratrol. The detected amounts ranged from 0.98 to 6.25 mg kg^?1 fresh weight with a mean value of 3.59 (white grapes) and 3.08 mg kg^?1 (red grapes), respectively.     

Cadmium Distribution in a Timberline Forest in the Hengduan Mountains in the Eastern Tibetan Plateau

In order to study the regional distribution, characterization, and possible source of Cadmium in the eastern Tibetan Plateau, samples of leaves, xylem, twigs, bark, and roots of timberline forest trees (fir or spruce) and soils at depths from 0 to 40 cm were collected in eight sites in Hengduan Mountains. According to Cd contents, organs and tissues were divided into three groups: the highest-level organ (roots: 0.237 mg · kg^?1), the high-level organ/tissue (bark: 0.183 mg · kg^?1 and twigs: 0.159 mg · kg^?1), and the low-level organ/tissue (xylem: 0.054 mg · kg^?1and leaves: 0.048 mg · kg^?1). Cd contents in Transect A were a little higher than Transect B. Sites near pollutant sources and high-levels are more sensitive to Cd pollution and accumulated more Cd, while Cd contents in sites far away from pollutant sources and low-level organ/tissue were relatively low. It is suggested that the eastern Tibetan Plateau has already been polluted by the influence of general circulation to some extent. Nevertheless, low Cd contents in some sites prove that high mountains may barricade Cd pollutants from monsoon.     

Characterisation of phenolic compounds of the ethyl acetate fraction from Tabernaemontana catharinensis and its potential antidepressant-like effect

This study evaluates the antidepressant-like effect and analysed the qualitative and quantitative 74 phenolic standards of ethyl acetate fraction from Tabernaemontana catharinensis leaves. Acute administration of fraction in mice reduced the immobility time in forced swimming and tail suspension tests confirming its antidepressant-like activity. The anti-immobility effect elicited by this fraction was prevented by the pretreatment of mice with PCPA (100 mg kg^?1), ketanserin (5 mg kg^?1), SCH 23,390 (0.05 mg kg^?1) or yohimbine (1 mg kg^?1). A sub effective dose of the fraction produced a synergistic effect with fluoxetine (5 mg kg^?1). Chromatographic analysis identified 4-hydroxybenzoic and p-coumaric acids in the ethyl acetate fraction from T. catharinensis. Capillary electrophoresis presented 7.34 ± 0.02 mg g^?1 of p-coumaric acid concentration in the fraction. Therefore, it is possible that antidepressant-like effect elicited by ethyl acetate fraction from T. catharinensis be dependent on the p-coumaric acid.     

Persistence of trifloxystrobin and tebuconazole in banana tissues and soil under the semi-arid climatic conditions of Karnataka,India

Trifloxystrobin and tebuconazole are used for control of Sigatoka leaf spot disease of banana. This study was conducted to evaluate residue persistence of the fungicides in/on banana fruit, other edible parts and soil after spray application of the combination formulation, Nativo 75 WG, at the standard dose, 87.5 + 175 and double dose, 175 + 350 g a.i. ha^?1. The fungicides were extracted from banana and soil with acetone, partitioned into dichloromethane and cleaned-up using activated charcoal for trifloxystrobin and primary/secondary amine (PSA) for tebuconazole samples. The limit of quantification of the method was 0.05 mg kg^?1 for both fungicides. Initial residues of trifloxystrobin were 0.444 and 0.552 mg kg^?1 in/on banana with peel (whole fruit), which reached <0.05 and 0.065 mg kg^?1 after 30 days from treatment at the standard and double doses, respectively. Tebuconazole residues were 0.636 and 960 mg kg^?1 initially and reduced to 0.066 and 0.101 mg kg^?1 after 30 days. Trifloxystrobin and tebuconazole degraded with the half-life of about 11 days. Trifloxystrobin or its metabolite was not detected in the fruit pulp. Tebuconazole being systemic in nature moved to the fruit pulp which was highest on the 3rd day (0.103 and 0.147 mg kg^?1) and remained for 15 days. Matured banana fruit, flower, pseudostem and field soil were free from fungicide residues. For consumption of raw banana 43 days pre-harvest interval (PHI) is required after treatment of the combination formulation. Therefore application of the fungicides towards maturity stage of the fruits may be avoided.     

Transfer of Metals from Soil to Crops in an Area near a Coal Gangue Pile in the Guqiao Coal Mine,China

A field survey was conducted to investigate the metal contamination in coal gangue, soils, and crops (rice and soybeans), and to evaluate the possible health risks to the local population through food chain transfer near a coal gangue pile in the Guqiao Coal Mine, China. Contamination levels of zinc, lead, cadmium, and copper in coal gangue, soils, and crops were measured, and bio-accumulation factors from soil to crops were determined; the health risks were calculated accordingly. Results showed that both coal gangue and soil contained high levels of cadmium (0.15 mg kg^?1and 0.20 mg kg^?1) exceeding the background value of the soil. The lead soil concentration was low (9.99 mg kg^?1), but lead in rice (0.38 mg kg^?1) exceeded the maximal permissible limit of 0.2 mg kg^?1. For some tissues of crops studied, there was a significant correlation between the bio-accumulation factor values and the corresponding soil metal concentrations that were best described by a power equation. Oral intake of zinc, cadmium, and copper through crops posed no health risk to local residents, although hazard indices for rice (0.87–2.88) and soybeans (0.06–0.09) suggested that ingestion of rice grains was unsafe for human health. Therefore, rice was inappropriate to be planted in the soil surrounding this coal mine.     

Ethanolic extracts of Moringa oleifera Lam.

This paper reports the evaluation of the antioxidant potential of the ethanolic extracts of the leaves (EL), flowers (EF), seed pods (EP) and seeds (ES) from Moringa oleifera Lam. The antioxidant potential was assessed, upon the addition of the extracts to fish oil, by means of the total extractable phenol content (TEP), the DPPH^· free radical scavenging efficiency and using pressurized differential scanning calorimetry (P-DSC). The results of TEP and DPPH^· showed that the ES extract does not present a potential to be used as an antioxidant additive, and it was thus discarded from the remaining analyses. Thus, the following treatments were prepared: pure fish oil, fish oil with BHT (100 mg kg^?1), fish oil with TBHQ (100 mg kg^?1) and fish oil with EL, EF and EP—all at the concentration of 100 mg kg^?1, in relation to the total extractable phenolics contained in each one of the extracts. The leaf and flower extracts displayed a protecting effect, with an increase in about 20 and 11 % of the OIT values, respectively. However, such protection was smaller than that conferred by the synthetic antioxidants utilized. As for the thermal analysis results, it was noticed that EL presented the highest thermal stability among the extracts.     

Biodegradation of imidacloprid in sandy loam soil by Bacillus aerophilus

A study of the biodegradation of imidacloprid in soil was carried out under laboratory conditions. Sandy soil samples were fortified with imidacloprid at 50, 100 and 150 mg kg^?1 along with 45 x 10⁷ colony forming units (cfus) of Bacillus aerophilus and the samples were compared with unamended soil. The samples were extracted with acetonitrile, cleaned up by treatment with primary secondary amine sorbent and graphitised carbon black. The residues of imidacloprid and its metabolites were analysed by high performance liquid chromatography. The parent compound, imidacloprid, was found to be more persistent in both the treatments. Among metabolites, the highest values were obtained for urea and olefin while 5-hydroxy, 6-chloronicotinic acid (6-CNA), nitrosimine and nitroguanidine (NTG) were also observed in all the treatments in amended soil. In case of unamended (control) soil, 6-CNA was found to be the most persistent metabolite followed by olefin, urea, 5-hydroxy, nitrosimine and NTG metabolites. Total imidacloprid residues for control soil samples followed first-order kinetics at 50 and 150 mg kg^?1 but in case of control imidacloprid fortified at 100 mg kg^?1, the total residues of imidacloprid and its metabolites followed pseudo-first-order kinetics. The respective half-life value for 50 mg kg^?1 was 25.08 days and 30.10 days for both 100 and 150 mg kg^?1. However, total imidacloprid residues followed pseudo-first-order kinetics for its applications at 50, 100 and 150 mg kg^?1 in sandy loam soil amended with B. aerophilus. The half-life values for 50, 100 and 150 mg kg^?1 were worked out to be 14.33, 15.05 and 18.81 days, respectively. With the use of B. aerophilus, the reduction percentage of initial applied dose imidacloprid in sandy loam soil was found to be higher in all the three doses as compared to that of the control samples.     

Comparison of an HPTLC method with the Reflectoquant assay for rapid determination of 5-hydroxymethylfurfural in honey

5-Hydroxymethylfurfural (HMF) was analyzed in 17 botanical varieties of honey from 12 countries. A recently developed high-performance thin-layer chromatographic (HPTLC) method was limited because of increased matrix effects at higher honey sample loading. Therefore, the method was modified to achieve higher sensitivity and eliminate matrix interference by use of rectangular application combined with a focusing step. The HPTLC results were compared with results from the new spectrophotometric Reflectoquant hydroxymethylfurfural assay. Both methods had quantification limits of 4 mg kg^?1 and were suitable for rapid quantification of HMF in honey at the strictest regulated level of 15 mg kg^?1. Comparable results were obtained for the 17 honey samples, with a mean deviation of 2.9 mg kg^?1 (15 %). The optimized HPTLC method was proved to be highly matrix-robust and was validated for the 17 different honey matrices (correlation coefficients ≥0.9994 (n?=?6), mean intra-day precision 3.2 % (n?=?3 within a plate; n?=?2 repeated within a day), mean inter-day precision 3.7 % (n?=?3), mean reproducibility over the whole procedure including sample preparation 4.1 % (n?=?2), and mean recovery 106.9 % (n?=?5 different concentrations; n?=?4 different honey matrices). Recovery for a range of different application volumes, and thus for different honey matrix loading, differed by only ≤4.2 %. HMF results when calculated by use of external calibration and by use of the standard addition method varied by 8.8 %. Both revealed that any matrix effect was minor and that the original matrix interference problem was successfully solved.

Dissipation rates of saisentong residues in fresh tobacco,tobacco powder and soil determined by high-performance liquid chromatography coupled with diode array detection

Two independent field trials were performed in Guizhou and Hunan, China in 2013 to investigate the dissipation and residue levels of saisentong in tobacco and soil. A novel and accurate method using high-performance liquid chromatography with diode array detection was developed and validated to determine saisentong levels in tobacco and soil. The average recovery of saisentong at fortification levels of 0.5, 2.5, 5.0 and 50.0 mg kg^?1 in fresh tobacco ranged from 75.92 to 107.40% with a relative standard deviation (RSD) of 0.94 to 7.55%, that at fortification levels of 0.5, 2.0 and 5.0 mg kg^?1 in tobacco powder ranged from 74.96 to 94.43% with a relative standard deviation (RSD) of 4.38 to 8.14%, and that at fortification levels of 0.1, 0.5 and 5.0 mg kg^?1 in soil ranged from 86.90 to 100.0% with an RSD of 1.38 to 4.62%. The limit of detection (LOD) of saisentong was 0.15 mg?kg^?1 in tobacco and 0.03 mg kg^?1 in soil, and the limit of quantification (LOQ) was 0.5 mg kg^?1 in tobacco and 0.1 mg kg^?1 in soil, respectively. For field experiments, the half-lives of saisentong in tobacco from Guizhou and Hunan were 5.9 and 1.6 days, respectively; those in soil were 14.7 and 12.0 days, respectively. The results suggest that the saisentong dissipation curves followed the first-order kinetic. The terminal residues of saisengtong in tobacco ranged from 0.5 to 9.39 mg kg^?1 at pre-harvest intervals (PHI) of 7, 14 and 21 days.     

Improving the Determination of Nitrovin in Feeds by Reversed-Phase LC with SPE

A simple reversed-phase liquid chromatographic method with ultraviolet detector (378 nm) for the determination of nitrovin in feeds was improved and validated. The mobile phase was a mixture of acetonitrile and 0.1% formic acid solution (v/v) in the ratio of 50:50 (v/v), and the flow rate was set at 1.2 mL min^?1. The extraction solution was a mixture of dimethyl formamide, acetonitrile and methanol (50:25:25, v/v), the sample was cleaned-up with reversed-phase solid phase extraction cartridge. The standard nitrovin was purified with crude nitrovin product by ethylene glycol monoethyl ether and identified by elemental analyzer. The limit of detection was 0.05 mg kg^?1 and the limit of quatification was 0.2 mg kg^?1 in feeds. The assay had satisfactory selectivity, recovery, linearity and precise repeatability and trueness.     

Removal of some radionuclides from contaminated solution using natural clay: bentonite

Clays and specially bentonite are widely used as natural adsorbents for wastewater treatment and as a barrier in landfills to prevent the contamination of subsoil and groundwater by leachates containing radioactive materials. The adsorption of four radionuclides, ¹³⁴Cs(I), ⁹⁰Sr(II), ¹³³Ba(II) and ¹⁵²Eu(III) by an Egyptian bentonite (Bent) and its modified Na⁺ form (Na-Bent) collected from a deposit within Alexandria governorate was investigated as a function of different parameters. The batch equilibrium technique was used and the kinetic results showed that the equilibrium was mostly reached within 10 min and the kinetic data fit well to the pseudo-second order model. The Langmuir model fits well the experimental data of all metals adsorption on Bent and Na-Bent except for adsorption of ¹³³Ba on Bent, while ¹⁵²Eu adsorption on Na-Bent fits better to the Freundlich model rather than to the Langmuir. Both Bent and Na-Bent fit well to the D-R model with adsorption energy of E > 8 kJ mol^?1 that means that the adsorption reaction is expected to be controlled by both cation exchange and surface complexation reactions. At lower concentrations, the values of distribution coefficient (K _d), follow the order of ¹⁵²Eu > ⁹⁰Sr > ¹³⁴Cs > ¹³³Ba for Bent and Na-Bent. The K _d of ¹⁵²Eu is higher than that of ¹³⁴Cs in Bent up to 150 mg L^?1. This order changes at higher concentration where the K _d of ¹³⁴Cs becomes higher than ¹⁵²Eu after 150 mg L^?1 for Bent and after 200 mg L^?1 for Na-Bent. Na-Bent is preferred than Bent for the uptake of ⁹⁰Sr and ¹³⁴Cs especially at high concentration.     

Residue dynamics of chlorpyrifos and cypermethrin in/on pomegranate (Punica granatum L.) fruits and soil

Study on the residue dynamics of chlorpyrifos and cypermethrin in/on pomegranate (Punica granatum L.) and soil was carried out by conducting supervised field trials as per good agricultural practices. A modified QuEChERS was used to extract the insecticides in pomegranate peel and aril and soil. The limit of quantification (LOQ) of chlorpyrifos and cypermethrin were 0.01 and 0.05 mg kg^?1, respectively. Residues of the insecticides remained on the fruit surface and movement to the edible part (aril) was not observed. The residues after treatment on fruit peel were 2.46 and 3.51 mg kg^?1 and 2.84 and 4.54 mg kg^?1 for chlorpyrifos and cypermethrin, respectively, from recommended and double dose treatments. Chlorpyrifos residues degraded faster compared to cypermethrin. The pre-harvest intervals (PHIs) of chlorpyrifos were 22 and 35 days and those of cypermethrin 50 and 73 days, respectively, at recommended and double dose treatments. In the experimental field soil after the second application chlorpyrifos residues were 0.21 and 0.46 mg kg^?1 and cypermethrin residues 0.15 and 0.36 mg kg^?1. At harvest, both pesticides showed residues below the LOQ. Based on this study, application of cypermethrin towards harvest may be avoided whereas chlorpyrifos can be applied with 22 days PHI.     

Concentration of arsenic in soil samples collected around the monazite processing facility, Thailand

Arsenic (As) in soil is a contaminant originated from human activities including pesticide use, mining and ore processing operations. In this work, As concentration in soil samples collected around the monazite processing facility, Pathum Thani, Thailand, was investigated. The collections of 24 soil samples were collected from the monazite processing area and 7 soil samples were collected from the control area without the processing activity of the same facility. Soils were digested with the mixture of HNO₃, HClO₄ and HF using a microwave digester. Inductively coupled plasma mass spectrometer (ICP-MS) equipped with an octopole reaction system (ORS) was used to determine the concentration of As in soils after the acid digestion. JB-3 (igneous rock) was the standard reference material used to check the accuracy of the method. It was found that the analytical results showed good agreement with the certified values. As concentration in soils collected from the monazite processing area ranged from 3.85 to 36.01 mg kg^?1 with the mean of 13.06 mg kg^?1. The concentration of As higher than the US EPA cancer soil screening level (22 mg kg^?1) was observed for only one sample. The control area showed As concentration varied from 9.59 to 14.19 mg kg^?1 with the mean of 11.97 mg kg^?1. The obtained results from this work were compared with the contaminated soil data of Amphoe Ron Phibun, Nakhon Si Thammarat, Thailand.     

Persistence and dissipation of fluopicolide and propamocarb on cabbage and soil under semi-arid climatic conditions

Persistence and dissipation of fluopicolide and propamocarb were studied on cabbage and soil as per good agricultural practices over a period of 2 years. A modified QuEChERS analytical method in conjunction with gas chromatography (GC) and GC–mass spectrometry was used for analysis of fluopicolide and its metabolite, 2,6-dichlorobenzamide, and propamocarb in cabbage and soil. The results of the method validation were satisfactory with recoveries within 74.5–100.81% and relative standard deviations 4.8–13.9% (n = 6). The limit of detection (LOD) and limit of quantification (LOQ) of both fluopicolide and 2,6-dichlorobenzamide were 0.003 µg mL^?1 and 0.01 mg kg^?1, respectively. The LOD and LOQ of propamocarb were 0.03 µg mL^?1 and 0.1 mg kg^?1, respectively. During 2013, the initial residue deposits of fluopicolide on cabbage were 0.60 and 1.48 mg kg^?1 from treatments at the standard and double doses of 100 and 200 g a.i. ha^?1 which dissipated with the half-life of 3.4 and 3.7 days. During 2014, the residues were 0.49 and 1.13 mg kg^?1 which dissipated with the half-life of 4.2 and 5.1 days. Propamocarb residues on cabbage were 5.36 and 12.58 mg kg^?1 in the first study (2013) and 4.85 and 10.26 mg kg^?1 in the second study (2014) from treatments at the standard and double doses of 1000 and 2000 g a.i. ha^?1, respectively. The residues dissipated with the half-life of 4–5.5 days. The preharvest interval, the time required for fluopicolide + propamocarb residues to dissipate below the maximum residue limits (notified by EU) at the standard dose, was 11.8 and 14 days during 2013 and 2014. Residue of 2,6-dichlorobenzamide was always <LOQ in cabbage. Residues of fluopicolide, 2,6-dichlorobenzamide and propamocarb were <LOQ in field soil at harvest.     

MSPD Procedure for Determination of Carbofuran, Pyrimethanil and Tetraconazole Residues in Banana by GC–MS

An extraction method based on matrix solid-phase dispersion was developed to determine carbofuran, pyrimethanil and tetraconazole in banana using gas chromatography–mass spectrometry. The best results were obtained using 2.0 g of banana, 1.0 g of silica as dispersant sorbent and n-hexane:ethyl acetate (1:4, v/v) as eluting solvent. The method was validated using banana samples fortified with pesticides at different concentration levels (0.05–2.0 mg kg^?1). Average recoveries (four replicates) ranged from 68 to 111%, with relative standard deviations between 6.6 and 20.5%. Detection and quantification limits for banana ranged from 0.02 to 0.05 and 0.05 to 0.10 mg kg^?1, respectively.