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1.
Persistence of dicofol residues in cotton lint seed, and soil   总被引:1,自引:0,他引:1  
A supervised field trial was conducted at the CCS Haryana Agricultural University, Hisar to assess the residues of dicofol on cotton, during Kharif season, 2008. Dicofol (Kelthane 18.5EC) was applied at 500 g a.i./ha (T(1)) and 1,000 g a.i./ha T(2)) after 105 days of sowing of cotton crop (Varity Cotton/H-1226). Soil samples were collected on 0 (1 h after treatment), 3, 7, 10, 15, 30, and 60 days after spray and cotton samples were collected at harvest. Samples were processed and residues were quantified by GC-ECD system equipped with capillary column. Limit of detection and limit of quantification (LOQ) were 0.001 and 0.010 mg kg(?-1), respectively, for soil and LOQ for cotton lint and seed was 0.020 mg kg(?-1). Initial residues of 0.588 and 1.182 mg kg(?-1) in soil reached below detectable level (BDL) of 0.010 mg kg(?-1) in T(1) and to the level of BDL (0.010 mg kg(?-1)) in T(2) at harvest (60 days after treatment). In 60 days, residues dissipated almost completely (100 and >99%) in both the treatments. Half-life period was calculated as 8.57 days at single dose and 8.69 days at double dose in soil. Residues of dicofol were detected in cotton lint to the levels of 0.292 and 0.653 mg kg(?-1) and in seed 0.051 and 0.090 mg kg(?-1) in T(1) and T(2) doses, respectively at harvest. Residues in cotton seed were below MRL value of 0.01 mg kg(?-1) in both the doses.  相似文献   

2.
The aim of the study was to investigate the transfer of toxic metals from honeybee workers (Apis mellifera L.) to bee honey in relation to the ecological state of the environment. The materials of the study consisted of samples of honeybee bodies and varietal honeys taken from the same apiary located in three areas: R1—urbanized (16), R2—ecologically clean (16) and R3—industrialized (15) of south-eastern Poland. The contents of 14 elements in all tested samples, including toxic metals (Cd, Pb, Hg, Al, Ni, Tl) as well as bioelements (K, Mg, Ca, Mn, Fe, Zn, Cu, Se), were analysed by the ICP-OES method with prior microwave mineralization. The concentrations of the majority of the studied elements, excluding aluminum and lead, were significantly higher in bee bodies than in honey samples (P?<?0.05). The pollution of bee bodies by toxic metals was dependent on the environmental cleanliness, and the most pollution was observed in the industrialized area. The bee body was the most effective barrier for Cd and Tl transfer to the honey, while the level of Ni was similar in both tested materials. The Al concentration was significantly higher in honey than bee bodies (14.81?±?24.69 and 6.51?±?5.83 mg kg?1, respectively), which suggests the possibility of secondary contamination of honey. The greatest sensitivity to heavy metal pollution was observed in honeydew honey compared to nectar honeys (P?<?0.05). It was proved for the first time that bees work as biofilters for toxic metals and prevent honey contamination.  相似文献   

3.
Regarding the hypothesis that neonicotinoid insecticides used for seed coating of agricultural crops - mainly corn, sunflower and seed rape - are related to the extensive death of honey bees, the phenomenon of corn seedling guttation has been recently considered as a possible route of exposure of bees to these systemic insecticides. In the present study, guttation drops of corn plants obtained from commercial seeds coated with thiamethoxam, clothianidin, imidacloprid and fipronil have been analyzed by an optimized fast UHPLC-DAD procedure showing excellent detection limits and accuracy, both adequate for the purpose. The young plants grown both in pots - in greenhouse - and in open field from coated seeds, produced guttation solutions containing high levels of the neonicotinoid insecticides (up to 346 mg L(-1) for imidacloprid, 102 mg L(-1) for clothianidin and 146 mg L(-1) for thiamethoxam). These concentration levels may represent lethal doses for bees that use guttation drops as a source of water. The neonicotinoid concentrations in guttation drops progressively decrease during the first 10-15 days after the emergence of the plant from the soil. Otherwise fipronil, which is a non-systemic phenylpyrazole insecticide, was never detected into guttation drops. Current results confirm that the physiological fluids of the corn plant can effectively transfer neonicotinoid insecticides from the seed onto the surface of the leaves, where guttation drops may expose bees and other insects to elevated doses of neurotoxic insecticides.  相似文献   

4.
Residues of flubendiamide and desiodo flubendiamide were studied following three applications of flubendiamide 480 SC at 7 days interval at 90 and 180 g a.i. ha(-1) in/on brinjal fruits. An average initial deposit of 0.33 and 0.61 mg kg(-1) of flubendiamide was observed respectively after application at single and double dosages. The residues of flubendiamide dissipated quickly at both the dosages, and after 3 days, the extent of dissipation was found to be about 76% and 79% at the single and double dosages, respectively. Brinjal fruit samples analysed at different time intervals did not show the presence of desiodo flubendiamide. The half-life of flubendiamide was observed to be 0.62 and 0.54 days at single and double dosages, respectively. The limit of determination of flubendiamide and desiodo flubendiamide was observed to be 0.05 mg kg(-1). Soil samples analysed after 15 days of the last application did not reveal the presence of flubendiamide and desiodo flubendiamide at their determination limit of 0.05 mg kg(-1). An assessment of the total intake of flubendiamide resulting through the consumption of brinjal fruits and its comparison with acceptable daily intake seems to be quite safe from consumer point of view.  相似文献   

5.
Possible bioaccumulation of pesticides in crop produce may cause ailing effect on animal and human. Thus there is a need to evaluate these chemicals in the soil and crop produce at harvest. Metsulfuron-methyl is a post-emergence herbicide. It is highly active to control broad-leaf weeds in cererals, pasture and plantation crops. Metsulfuron-methyl was applied at 3, 4, 5, and 8 g a.i. ha(-1) rates, after 30 days of sowing in wheat as post-emergence herbicide. Soil samples treated with metsulfuron-methyl were collected after 30 and 60 days along with control and at harvest after herbicide application and analyzed for residues by High Performance Liquid Chromatography (HPLC) using photo diode array detector at 220 nm. Wheat grains and straw samples were sampled at harvest. At harvest the residue level of metsulfuron-methyl in soil was found below the detection limit at 3-5 g a.i. ha(-1) application rates and 0.002 microg g(-1) at 8 g a.i. ha(-1), respectively. No residues of metsulfuron-methyl were detected in wheat grains at 3-4 g a.i. ha(-1) rates. However 0.002 microg g(-1) residues were detected in wheat straw at 5 and 8 g a.i. ha(-1) application rates. It can be concluded that metsulfuron-methyl application at 3-4 g a.i. ha(-1) can be safely applied to the wheat crop as post-emergence herbicide.  相似文献   

6.
In a field study carried out at three different locations, the dissipation of spiromesifen on cotton and chili was studied and its DT50, and DT99 were estimated at each location. Spiromesifen was sprayed on chili at 96 and 192 g a.i. ha−1 and cotton at 120 and 240 g a.i. ha−1. Samples of chili fruits were drawn at 0, 1, 3, 5, 7, 10, 15, 21, 30 days after treatment and that of cotton seed and lint at first picking and harvest. Soil samples were drawn 30 days after treatment from 0 to 15 and 15 to 30 cm layer. Quantification of residues was done on GC–MS in Selected Ion Monitoring (SIM) mode in mass range 271–274 m/z. The LOQ of this method was found 0.033 μg g−1, LOD being 0.01 μg g−1. The DT50 of spiromesifen when applied at recommended doses in chili fruits was found to be 2.18–2.40 days. Ninety-nine percent degradation was found to occur within 14.5–16.3 days after application. Residues of spiromesifen were not detected in cotton seed and lint samples at the first picking. In soil, no residues of spiromesifen were detectable 15 days after treatment.  相似文献   

7.
采用毛细管柱气相色谱-质谱选择离子检测技术,结合加速溶剂萃取和凝胶渗透色谱净化方法,分析土壤中的6种酞酸酯类(PAFs)化合物。结果表明,土壤中6种PAEs检出限在14—42μg/kg间,加标平均回收率为65.5%~104.4%,相对标准偏差为5.19%~9.61%。方法具有操作简便、纯化效果好和对环境友好的特点,且具有很强的实用性。  相似文献   

8.
浓缩果汁中氰戊菊酯和溴氰菊酯农药残留测定方法研究   总被引:5,自引:0,他引:5  
叶菁 《干旱环境监测》2008,22(2):117-119
应用柱层析净化技术和毛细管气相色谱法,采取恒温模式和不分流进样方式,在μ-ECD检测器上测定浓缩果汁样品中氰戊菊酯和溴氰菊酯农药的残留组份。测定结果表明:2种农药分离效果较好,其线性范围较宽(0.1-10mg/L,可达ppm级),在规定浓度范围内与峰面积呈良好的线性关系;方法的最低检测限氰戊菊酯为0.560μg/L,溴氰菊酯为0.702μg/L,相对标准偏差均小于10%(5.78%-8.62%),其加标回收率在89.2%-103.6%之间。研究建立的方法简便、快速、经济,具有良好的灵敏度、精密度和准确度,可以满足浓缩果汁样品中菊酯类农药的残留检测要求。  相似文献   

9.
A field experiment was conducted at Anand Agricultural University, Anand during Sept-Dec, 2009 to study the rate of degradation of flubendiamide in/on brinjal fruits following foliar application of Fame 480 SC at 90 (standard dose) and 180 (double dose) g a.i. ha(?-1). The residues estimated using HPLC revealed persistence of flubendiamide in/on brinjal till 3rd and 7th day after the last spray at standard and double dose, respectively. The residues of flubendiamamde were reported as parent compound, and no desiodo metabolite was detected. The initial deposits of 0.17 and 0.42 μg g(?-1) in/on brinjal fruits reached below determination level of 0.05 μg g(?-1) on the 5th and 10th day at standard and double dose, respectively. The half life of flubendiamide on brinjal fruits ranged from 2.68 to 2.55 days. Soil samples analyzed on the 15th day after the last spray revealed residues at below determination level (0.05 μg g(?-1)) at either dose of application.  相似文献   

10.
A microwave-assisted solvent extraction (MASE) technique was developed for the quantitative extraction of gasoline- and diesel-range petroleum hydrocarbons (PHs) from soil and marine sediment samples. The influence of different extracting solvents, extraction temperature and duration of extraction on the recoveries of PHs was evaluated using a two-level orthogonal array design (OAD) with a OA8(27) matrix. Gas chromatographic-mass spectrometry (GC-MS) in multiple selective ion monitoring (MSIM) mode was used for the analysis of the PHs in environmental samples. The spiking range of the PHs in the environmental samples was between 1 to 1000 g/g. Good recoveries (>80%) could be obtained for most of the PHs using the optimum MASE conditions. The limit of detection (LOD) achieved by the GC-MS-MSIM was 0.02 g/g. A preliminary survey for the levels of PHs in marine sediment and soil samples from different parts of Singapore was carried out using the method.  相似文献   

11.
建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1~100 ng/mL(BDE-209为10~1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004~0.1 ng/g,方法回收率为75%~110%,方法精密度为2.4%~15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。  相似文献   

12.
The portion-dilution model is a parametric restatement of the conventional view of animal pollination; it predicts the level of pollinator-mediated gene dispersal. In this study, the model was applied to white clover (Trifolium repens) and its most frequent pollinator, the honeybee (Apis mellifera). One of the three parameters in the portion-dilution model is the mean number of flowers a pollinator visits in one foraging bout. An alternative method to estimate this parameter was developed that was not depending on pollinator hive-seeking behaviour. The new estimation method, based on nectar collection, seems to be a good alternative, when reliable observation on visiting behaviour of pollinators is not possible. The gene flow in white clover was modelled. Where fields were assumed to be well separated, and only a low fraction of bees travelled between fields, the gene flow was estimated to be 0.7%, but subjected to large uncertainty. In a worst case scenario with adjacent fields—one with a genetically modified (GM) T. repens cultivar and the other with a conventional T. repens cultivar—and where all arriving bees were expected to transfer GM pollen, the median gene flow was modelled to be 7% with an estimated 95% percentile of 70%. The results show that the European Union threshold limit of 0.9% GM admixture for food and feed will likely be exceeded at times and especially organic farmers that do not accept GM admixture and often have clover and clover–grass fields might face challenges with admixture of GM.  相似文献   

13.
The development of easy-to-use and rapid-monitoring immunoassay methods for organic environmental pollutants in a class-selective manner is a topic of considerable environmental interest. In this work, a heterologous competitive indirect enzyme-linked immunosorbent assay (ciELISA) based on a monoclonal antibody (MAb) with broad-specificity for organophosphorus pesticides (OPs) was applied to the detection of O,O-diethyl and O,O-dimethyl OPs in water samples. The ciELISA conditions were carefully optimized to obtain a three to five-fold improvement of sensitivity for most OPs, and thirteen OPs were determined at concentrations ranging from 0.017 to 30 ng mL(-1). The determination of spiked environmental water samples showed average recoveries from 81.5% to 115.1%, with the coefficient of variation (CV) ranging from 6.1% to 20.9%, which showed satisfactory reproducibility of the developed ciELISA. To overcome the negative aspect of broad-specificity immunoassays not providing qualitative and quantitative analysis of individual OPs in blind samples, we used "percent inhibition rate" to make the developed ciELISA a semi-quantitative method, which allows the monitoring of positive samples from hundreds of negative samples. The determination of OPs in blind water samples by the developed ELISA with confirmation by HPLC-MS/MS analysis demonstrated that the assay is ideally suited as a screening method for OP residues prior to chromatographic analysis.  相似文献   

14.
Interest in possible sources of perchlorate (ClO4) that could lead to environmental release has been heightened since the Environmental Protection Agency placed this anion on its Contaminant Candidate List for drinking water. Although recent investigations have suggested that fertilizers are minor contributors to environmental perchlorate contamination overall, there is still interest in screening commercial products for possible contamination and quantitating perchlorate when it is found. Ion chromatography (IC) has been used for this application owing to its speed, low detection limits, widespread availability, and moderate ruggedness relative to other techniques. However, fertilizer matrixes complicate the IC analysis relative to potable water matrixes. In this study, the performance of poly(vinyl alcohol) gel resin IC columns (100 mm and 150 mm) was evaluated for fertilizer matrixes using method EPA/600/R-01/026. The NaOH eluent included an organic salt, sodium 4-cyanophenoxide. Detection was by suppressed conductivity. A set of 55 different field samples representing 48 products and previously used by the EPA to assess occurrence of perchlorate in fertilizers (EPA/600/R-01/049) was reanalyzed on the 150 mm column. The 100 mm column was used to further investigate the positive hits. Both columns gave satisfactory performance in fertilizer matrixes, with spike recoveries (+/- 15%), assured reporting levels (0.5-225 microg g(-1) except for one at 1,000 microg g(-1)), accuracy (relative error < 30% always and most < 15%), and precision [injection-to-injection reproducibility < 3% relative standard deviation (RSD)] comparable to those reported in other studies. Performance did not vary substantially between column lengths. Lastly, the results of this investigation provided further evidence in support of the conclusions that had been reached previously by the EPA on the occurrence of perchlorate in fertilizers.  相似文献   

15.
Polychlorinated biphenyl (PCB) and organochlorine pesticide (OCP) levels in fat tissue of red and fallow deer (Cervus elaphus L. and Dama dama L.) from two inland and an Adriatic area were established. Of 17 analysed PCBs, PCB-28, PCB-138, PCB-153, PCB-180 and PCB-118 were found in all samples, whilst PCB-101 and PCB-170 were found in more than 50% of samples. They ranged between 0.03 and 5.98 ng g(-1) fat weight. Of seven analysed OCPs, HCB, γ-HCH and 1,1-dichloro-2,2-di(4-chlorophenyl)ethylene (DDE) were found in all samples, whilst β-HCH was found in more than 50% of samples. They ranged between 0.17 and 22.14 ng g(-1) fat weight. The dominating compounds were DDE, PCB-138, PCB153, PCB-118 and PCB-180. According to the Duncan multistage test, the levels of PCB-138, PCB-153, PCB 170 and PCB-180 were significantly higher in perirenal fat samples of specimens taken from the Adriatic area. DDE was significantly higher in the inland deer samples. Some species differences were determined and were mostly related to higher PCB and β-HCH levels in fallow deer samples and higher DDE levels in red deer samples. No sex difference was established. As for age, significantly higher levels of PCB-118 and PCB-52 were found in fawns.  相似文献   

16.
以洪泽湖中6种代表性生物为研究对象,采用超声波法提取样品中硝基苯类化合物,用凝胶色谱净化、浓缩,气相色谱/质谱联用法测定。该法与索氏提取法在同等试验条件下进行加标回收试验,前者回收率高且稳定,简便可行。方法检出限为0.008μg/g~0.030μg/g,平均加标回收率为76.5%~109%,重复测定3次的RSD为1.5%~13.0%。  相似文献   

17.
A simple and fast solid phase extraction procedure was developed to pre-concentrate traces of Cu and Zn prior to their determination in honey samples by flame atomic absorption spectrometry. The sample preparation included dissolution of honey samples and the passage (at 20 ml/min) of resulting 10 % m/v solutions (100 ml) through Dowex 50W?×?8-400 resin beds in order to quantitatively retain Cu and Zn and separate them from the glucose and fructose matrix. Enriched Cu and Zn traces were recovered with 5.0 ml of a 3.0 mol/l HCl solution and quantified by flame atomic absorption spectrometry. The procedure proposed was used to analyze sixty nine commercially available and freshly ripened honey samples coming from the Lower Silesia region (Poland). It enabled to measure Cu and Zn within the range of 0.01–1.42 and 0.03–15.38 μg/g, respectively, with precision better than 4 %. Accuracy, assessed on the basis of the recovery test and the comparison of results with those obtained using wet digestion and inductively coupled plasma optical emission spectrometry, was ranged from ?4 % to +6 %. Detection limits of Cu and Zn achieved with this method were 5 and 7 ng/g, respectively.  相似文献   

18.
Fused-silica-lined (FSL) canisters and SUMMA polished (SUMMA) canisters were compared for the recoveries and the stabilities of 58 volatile organic compounds (VOCs) at low ppbv (volume/volume) levels under various humidified conditions using a three-stage preconcentration method followed by GC-MS analysis. The target VOCs included non-polar VOCs (e.g. halogenated hydrocarbons and aromatic hydrocarbons) and polar VOCs (e.g. alcohols, ketones, esters, ethers, nitriles and thiols). The three-stage preconcentration method was initially optimized for simultaneous analysis of non-polar and polar VOCs because determination of canister stability is dependent on the accuracy of analytical measurements. The method showed good linearity over the concentration range from 1 to 25 ppbv for all target analytes, and the correlation coefficients were higher than 0.9974. The method detection limits ranged from 0.023 to 0.39 ppbv. The test mixtures loaded in both type of canisters (n = 3) had concentrations of 1.7-2.5 ppbv per compound at ambient pressure under various humidified conditions (%RH = 1.6, 8.0, 27, 39, 53 and >99% with excess water present). All canister samples were initially analyzed on day 0 (after 6-12 h). The effect of competitive adsorption of water vapor and polar VOCs on active sites of interior surface was remarkably observed for SUMMA canisters. Polar VOCs had a greater requirement for water vapor to be present. The RH percentages that ensured good recovery on day 0 were RH > 8% for non-polar VOCs and RH > 27% for polar VOCs (except alcohols under the condition of RH > 99%). All thiols were not recovered from SUMMA canisters under all conditions. FSL canisters showed good recoveries of more than 86% for all VOCs under all conditions on day 0 (except alcohols under the condition of RH > 99%). The recoveries of alcohols in both canisters under the condition of RH > 99% displayed relatively low recoveries in the range 25-76% because of the partitioning effect into condensed water. The canister samples under the conditions of RH 8.0, 27, 53 and > 99% were analyzed for the stability test on days 3, 7, 14 and 28 after loading. All non-polar VOCs were reasonably stable in the FSL canisters under all examined conditions over 28 days. However, several polar VOCs that have relatively lower vapor pressure, e.g. MIBK, butyl acetate and alcohols except ethanol, showed unstable characteristics under relatively dry conditions (RH 8 and 27%) during 28 days. RH > 53% was needed to ensure good stabilities of all analytes except thiols with the recoveries of > 80% over 28 days for both canisters. Although the FSL canister showed good recoveries of more than 86% for thiols on day 0, drastic degradations were observed after day 3 and they were not detected after day 14.  相似文献   

19.
Supervised field trials were conducted at the research farms of four agricultural universities located at different agro-climatic zones of India to find out the harvest time residues of flubendiamide and its des-iodo metabolite on pigeon pea (Cajanus cajan) during the year 2006-2007. Two spray applications of flubendiamide 20 WDG at 50 g (T(1)) and 100 g (T(2)) a.i./ha were given to the crop at 15-days interval. The foliage samples at different time intervals were drawn at only one location, however, the harvest time samples of pigeon pea grain, shell, and straw were drawn at all the four locations. The residues were estimated by HPLC coupled with UV-VIS variable detector. No residues of flubendiamide and its des-iodo metabolite were found at harvest of the crop at or above the LOQ level of 0.05 μg/g. On the basis of the data generated, a pre-harvest interval (PHI) of 28 days has been recommended and the flubendiamide 20 WDG has been registered for use on pigeon pea by Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India and the MRL has been fixed by Ministry of Health and Family Welfare, Government of India under Prevention of Food and Adulteration as 0.05 μg/g on pigeon pea grains.  相似文献   

20.
Adsorbent sampling with analysis by thermal desorption, gas chromatography and mass spectrometry (TD/GC/MS) offers many advantages for volatile organic compounds (VOCs) and thus is increasingly used in many applications. For environmental samples and other complex mixtures, the MS detector typically is operated in the scan mode to aid identification of co-eluting compounds. However, scan mode does not achieve the optimal sensitivity, thus compounds occurring at low concentrations may not be detected. This paper develops and evaluates the application of a more sensitive TD/GC/MS method using selective ion monitoring (SIM) that is applicable to VOC mixtures found in ambient and indoor air. Based on toxicity and prevalence, 94 VOCs (including terpenes, aromatic, halogenated and aliphatic compounds) were selected as target compounds. Two analytical methods were developed: a conventional full scan method for ions from 29 to 270 m/z; and a SIM method using 16 time windows and different ions selected for the compounds in each window. Both methods used the same Tenax GR adsorbent sampling tubes, TD and GC parameters, and target and qualifier ions. Laboratory tests determined calibrations, method detection limits (MDLs), precisions, recoveries and storage stability. Field tests compared scan and SIM mode analyses for duplicate samples of indoor air in 51 houses and outdoor air at 41 sites. Statistical analyses included the development of error/precision models. The laboratory tests showed that most compounds demonstrated excellent precision (<10% for concentrations exceeding approximately 0.5 microg m(-3)), good linearity, near identical calibrations for scan and SIM modes, a wide dynamic range (up to 1500 microg m(-3)), and negligible storage losses after 1 month (7 compounds showed moderate losses). SIM mode MDLs ranged from 0.004 to 0.27 microg m(-3), representing a modest (1.1 to 22-fold) improvement compared to scan mode. However, in field tests the SIM method detected significantly more compounds (e.g., styrene and chloroform). Error models fit most compounds and allow quantification of errors at selected percentiles. Overall, while the new SIM method is somewhat time-consuming to develop, it offers greater sensitivity and maintains the high selectivity of traditional scan methods.  相似文献   

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