Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna)

A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy–precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01–1.0 μg mL^?1 for OCs and OPs and 0.05–2.5 μg mL^?1 for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70–120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg^?1, and the LOQs were determined as 0.01-0.049 mg kg^?1. The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India.     

铈改性净水污泥除磷效能与机理分析

磷酸盐含量是控制水环境质量的重要标准之一,吸附是一种高效、清洁和经济的除磷技术。采用铈改性净水污泥吸附去除磷酸盐,考察了铈负载量、投加量、pH、共存离子等因素对吸附磷酸盐的影响,探讨了可能的吸附机理及吸附材料循环再生能力。结果表明,铈改性净水污泥吸附磷酸盐过程符合拟二级动力学和Freundlich吸附等温线,最大吸附量为69.43 mg·g⁻¹,吸附速率受内扩散、边界层效应等多重因素的限制。在Cl⁻、NO₃⁻、CO₃²⁻、SO₄²⁻等共存离子干扰下,铈改性净水污泥具备选择性吸附磷酸盐的能力。在进行5次吸附-解吸循环后,吸附材料对磷酸盐的去除率下降了25.4%。吸附机制主要为磷酸盐与羟基以及含铈基团的静电吸引和配体交换。     

Extending the EU Renewable Energy Directive sustainability criteria to solid bioenergy from forests

Solid bioenergy from forests plays — and is expected to continue to play — a key role to fulfil the renewable energy targets at the European Union level. When the Renewable Energy Directive was enacted, sustainability criteria were incorporated solely for biofuels and bioliquids. Sustainability criteria for solid bioenergy are also needed in order to prevent wood and primary forest residues from posing additional environmental risks to ecosystems. Acknowledging this, the European Commission has been working on extending the biofuels and bioliquids provisions to solid biomass. An internal draft was circulated in August 2013 which addressed the ways to both balance and mitigate the risks in three main topics: biodiversity; sustainable forest management; and greenhouse gases. This paper presents a set of criteria and indicators, developed during workshops with experts from Governments, scientific institutions, businesses and NGOs, that may be considered by the EU to assure that solid biomass from forests is obtained in an environmentally sustainable way.     

壳聚糖对菠菜中毒死蜱和乐果的降解作用（Effects of Spraying Chitosan on Degradation of Chlorpyrifos and Dimethoate Residues in Spinach）

在露地栽培条件下,研究了叶面喷施壳聚糖水溶液对菠菜中毒死蜱和乐果的降解作用.结果表明,叶面喷施不同浓度的壳聚糖(50、100、200、400mg·L-1)可有效降低菠菜中毒死蜱和乐果残留量,其中较低浓度壳聚糖能更有效地降低菠菜中毒死蜱、乐果的残留量.50mg·L-1壳聚糖使菠菜中毒死蜱残留量较对照降低40.2%,安全间隔期缩短2.07d;100mg·L-1壳聚糖使菠菜中乐果残留量较对照降低46.9%,安全间隔期缩短0.5d.壳聚糖作为一种有机磷农药降解剂应用于蔬菜生产是可行的.     

Soil bound residues of carbaryl and 1‐naphthol: Release and mineralization in soil,and uptake by plants

Abstract

¹⁴C‐carbaryl and ¹⁴C‐1‐naphthol form soil bound residues which get partially released when barley was grown. ¹⁴C‐residues could be detected in both shoot and root in the case of carbaryl treatment while only roots showed ¹⁴C‐residues in the case of 1‐naphthol. Flooding enhanced release of the bound residues while soil amendment did not. There was greater mineralization of bound residues of carbaryl than that of 1‐naphthol. Rice straw amendment enhanced mineralization.     

Degradation of telone II in contaminated and noncontaminated soils

Abstract

Degradation of the nematicide Telone II (cis‐ and trans‐1,3‐dichloropropene comprise the active ingredients) in soil was studied using ¹⁴C‐l,3‐dichloropropene (DCP) along with soil samples collected from a field test site near Quincy, Florida. A mixed bacterial culture isolated from the soil in the presence of a second carbon source, glucose or yeast extract, completely degraded ¹⁴C‐DCP to ¹⁴CO₂, water‐soluble products, and microbial mass. ¹⁴C‐DCP in soil was also degraded to ¹⁴CO₂. After 28 days of incubation, the labeled chemical was completely degraded to ¹⁴CO₂, water‐soluble metabolites, bound‐residues, and possibly some microbial mass. Little or no difference was observed in the degradation of ¹⁴C‐DCP in soil samples collected one week prior to field application of Telone II, or two weeks and two years after application.     

14C‐dimethoate residues in olive oil during oil processing

Abstract

An olive tree was treated twice in the field with ¹⁴C‐dimethoate (237.7 (μCi, 2.4 g) and ¹⁴C residues were determined in the olive fruits at harvest. The fruits were crushed and pressed to extract the crude oil, then refined by neutralization, bleaching and deodorization. The crude oil contained 14.1% of the total ¹⁴C in the olive fruits. Neutralization resulted in a reduction of ¹⁴C by about 50% of the total ¹⁴C residues in oil. Bleaching and deodorization processes further reduced the ¹⁴C residues and the refined oil contained 31.6% (which corresponds to 4.4% of ^I4C residues of the total ¹⁴C in olive fruits) of the total ¹⁴C in the crude oil. Industrially extracted crude oil was fortified with ¹⁴C‐dimethoate at 1.8 mg kg^‐1 (0.02 μCi) level and subjected to the same refining process. A sharp decrease in the amount of ¹⁴C was observed by neutralization and the amount of ¹⁴C remaining in the refined oil was about 7.3% of the total ^l4C in the crude fortified oil. The data suggest that the ¹⁴C residues in the aged and the fortified oil amples were not of the same nature. The terminal ¹⁴C residue in the refined oil obtained from the field experiment did not contain dimethoate and/or its oxon.     

Cyhalofop‐p‐butyl mobility and distribution of residues in soil at various depths

This study was conducted to evaluate cyhalofop‐p‐butyl mobility in a sandy loam soil and subsequent distribution of residues at various depths under field conditions. Soil samples were taken from 0 to 150 cm depths at 3–90 d after rains in lysemeter of 1 and 2 m depths. Cyhalofop‐p‐butyl application at two rates and subsequent precipitation had a significant impact on soil, physico‐chemical properties and herbicide mobility. Precipitation caused substantial mobility of cyhalofop‐p‐butyl in the soil and 1.1–7.6 μg L^?1 of cyhalofop‐p‐butyl was found in leachates. Cyhalofop‐p‐butyl residues in the leachates were probably due to preferential flow through the soil. Cyhalofop‐p‐butyl residues were detected in significant amounts from the soil up to 10 d, later, residues were found below the detection limit but its three transformation products viz., cyhalofop acid, diacid, and phenol were detected.     

Photomirex: A teratogenicity and tissue distribution study in the rabbit

Abstract

Adult New Zealand white does were intubated orally with single daily doses of 0, 5, or 10 mg of photomirex (8‐monohydromirex) per kg body weight from the 6th through to the 18th day of gestation. Pregnancies were interrupted at term by cesarian section and fetuses removed and evaluated by following routine teratologic methods. Both maternal and fetal tissues were analyzed for residues of photomirex. None of the treated does showed any sign of toxicity. Except for a significant reduction in the mean fetal weight of the 10 mg/kg group all other parameters which evaluated fetal survival and fetal development were within the control range. Photomirex was found in all tissues examined. In the doe, the highest levels were found in fat followed by liver, kidney, spleen, heart, brain and blood. Photomirex was readily transferred across the placenta and accumulated in the fetus. However, in the fetus the highest levels were found in the heart, followed by liver, brain and blood. There were no teratogenic effects at the doses used in this study.     

Influence of humic fractions on retention of isoproturon residues in two Moroccan soils

The influence of different fractions of soil organic matter on the retention of the herbicide isoproturon (IPU) has been evaluated. Water and methanol extractable residues of ¹⁴C labeled isoproturon have been determined in two Moroccan soils by β -counting–liquid chromatography. The quantification of bound residues in soil and in different fractions of soil humic substances has been performed using pyrolysis/scintillation-detected gas-chromatography. Microbial mineralization of the herbicide and soil organic matter has been also monitored. Retention of isoproturon residues after 30-days incubation ranged from 22% to 32% (non-extractable fraction). The radioactivity extracted in an aqueous environment was from 20% to 33% of the amount used for the treatment; meanwhile, methanol was able to extract another 48%. Both soils showed quantities of bound residues into the humin fraction higher than humic and fulvic acids. The total amount of residues retained into the organic matter of the soils was about 65 % of non-extractable fraction, and this percentage did not change with incubation time; on the contrary, the sorption rate of the retention reaction is mostly influenced by the clay fraction and organic content of the soil. Only a little part of the herbicide was mineralized during the experimental time.