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1.
A modified LC-MS method for the analysis of mepiquat residue in wheat, potato, and soil was developed and validated. A hydrophilic interaction liquid chromatographic column has been successfully used to retain and separate the mepiquat. Mepiquat residue dynamics and final residues in supervised field trials at Good Agricultural Practice (GAP) conditions in wheat, potato, and soil were studied. The limits of quantification for mepiquat in all samples were all 0.007 mg kg?1, which were lower than their maximum residue limits. At fortification levels of 0.04, 0.2, and 2 mg kg?1 in all samples, recoveries ranged from 77.5 to 116.4 % with relative standard deviations of 0.4–7.9 % (n?=?5). The dissipation half-lives (T 1/2) of mepiquat in soil (wheat), wheat plants, soil (potato), and potato plants were 4.5–6.3, 3.0–5.6, 2.2–4.6, and 2.4–3.2 days, respectively. The final residues of mepiquat were below 0.153 mg kg?1 in soil (wheat), 0.052–1.900 mg kg?1 in wheat, below 0.072 mg kg?1 in soil (potato), and below 1.173 mg kg?1 in potato at harvest time. Moreover, pesticide risk assessment for all the detected residues was conducted. A maximum 0.0012 % of acceptable daily intake (150 mg kg?1) for national estimated daily intake indicated low dietary risk of these products.  相似文献   

2.
Dissipation and decontamination of chlorantraniliprole (Coragen 18.5 SC) in brinjal and okra fruits were studied following field application at single and double doses of 30 and 60 g ai ha?1, and the residues of the insecticide was estimated using LC-MS/MS. Initial residues of chlorantraniliprole at single and double doses on the fruits of brinjal were 0.72 and 1.48 mg kg?1, while on okra fruits, the residues were 0.48 and 0.91 mg kg?1, respectively. The residues reached below detectable level of 0.01 mg kg?1 on the 10th day. Half-life of chlorantraniliprole at 30 and 60 g ai ha?1 on brinjal was 1.58 and 1.80 days with the calculated waiting period of 0.69 and 2.38 days, whereas on okra, the values were 1.60 and 1.70 and 0 and 1.20 days, respectively. The extent of removal of chlorantraniliprole using simple decontaminating techniques at 2 h and 3 days after spraying was 40.99–91.37 % and 29.85–89.12 %, respectively, from brinjal fruits and 47.78–86.10 % and 41.77–86.48 %, respectively, from okra fruits.  相似文献   

3.
The metabolic degradation and persistence of imidacloprid in paddy field soil were investigated following two applications of imidacloprid at 20 and 80 g a.i. ha?1 at an interval of 10 days. The soil samples were collected at various time intervals. The limit of quantification for the analysis of imidacloprid and its metabolites was obtained at the concentration of 0.01 mg kg?1. The initial deposits of total imidacloprid were found to be 0.44 and 1.61 mg kg?1 following second applications. These residues could not be detected after 60 and 90 days following second applications of imidacloprid at lower and higher dosages, respectively. In soil, urea metabolite was found to be the maximum, followed by olefine, nitrosimine, 6-chloronicotinic acid, 5-hydroxy and nitroguanidine. The half-life values (t 1/2) of imidacloprid were worked out to be 12.04 and 11.14 days, respectively, when applied at lower and higher doses, respectively.  相似文献   

4.
A field study was conducted to determine persistence and bioaccumulation of oxyflorfen residues in onion crop at two growth stages. Oxyfluorfen (23.5% EC) was sprayed at 250 and 500 g ai/ha on the crop (variety, N53). Mature onion and soil samples were collected at harvest. Green onion were collected at 55 days from each treated and control plot and analyzed for oxyfluorfen residues by a validated high-performance liquid chromatography method with an accepted recovery of 78–92% at the minimum detectable concentration of 0.003 μg g???1. Analysis showed 0.015 and 0.005 μg g???1 residues of oxyfluorfen at 250 g a.i. ha???1 rate in green and mature onion samples, respectively; however, at 500 g a.i.ha???1 rates, 0.025 and 0.011 μg g???1 of oxyfluorfen residues were detected in green and mature onion samples, respectively. Soil samples collected at harvest showed 0.003 and 0.003 μg g???1 of oxyfluorfen residues at the doses 250 and 500 g a.i. ha???1, respectively. From the study, a pre-harvest interval of 118 days for onion crop after the herbicide application is suggested.  相似文献   

5.
Chlorantraniliprole, an anthranilic diamide insecticide with novel mode of action, is found effective against several lepidopteran as well as coleopteran, dipteran, and hemipteran pests. The present studies were carried out to study the persistence pattern of chlorantraniliprole on sugarcane field soil following application of granule formulation. The residues of chlorantraniliprole were estimated using high performance liquid chromatograph (HPLC) and confirmed by liquid chromatograph-mass spectrometry (LC-MS/MS). Following application of chlorantraniliprole (Ferterra 0.4G) at 100 and 200 g a.i. ha?1, the average initial deposits of chlorantraniliprole were observed to be 0.88 and 1.59 mg kg?1, respectively. These residues dissipated below the limit of quantification (LOQ) of 0.01 mg kg?1 after 56 days of the application of insecticides at both the dosages. The half-life values (t 1/2) of chlorantraniliprole were worked out to be 8.36 and 8.25 days, at recommended and double the recommended dosages, respectively.  相似文献   

6.
Two-year field trials were performed at two experimental sites to investigate dissipation and terminal residues of propamocarb in ginseng root, stem, leaf, and soil by high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Mean recoveries ranged from 80.5 to 95.6 % with relative standard deviations (RSDs) of 5.5–9.1 % at fortified levels of 0.01, 0.02, 0.05 and 0.20 mg kg?1. The half-lives of propamocarb were 5.00–11.36 days in root, 5.07–11.46 days in stem, 6.83–11.31 days in leaf and 6.44–8.43 days in soil. The terminal residues of propamocarb were below the maximum residue limits (MRLs) of EU (0.20 mg kg?1) and South Korea (0.50 mg kg?1 in fresh ginseng and 1.0 mg kg?1 in dried ginseng) over 28 days after last spraying at recommended dosage. The results provide a quantitative basis for establishing the MRL and give a suggestion of safe and reasonable use of propamocarb in ginseng.  相似文献   

7.
The persistence and metabolism of imidacloprid in soil under sugarcane were studied following application of imidacloprid at 20 and 80 g active ingredient (a.i.) ha?1. Soil samples were collected at different time intervals (7, 15, 30, 45, 60 and 90 days after application), and the residues of imidacloprid and its metabolites (6-chloronicotinic acid, nitrosimine, imidacloprid-NTG, olefin, urea and 5-hydroxy) were quantified by high-performance liquid chromatography. In soil, the total imidacloprid residues were mainly constituted by the parent compound followed by 6-chloronicotinic acid, nitrosimine and imidacloprid-NTG metabolites. Maximum residues of imidacloprid and its metabolites were 4.29 and 7.81 mg kg?1 in soil samples collected 7 days after the application of imidacloprid at 20 and 80 g a.i. ha?1, respectively. At both doses, these residues declined to below the detectable limit in soil after 90 days of application. Olefin, urea and 5-hydroxy metabolites were not detected in soil. Dissipation of total imidacloprid residues did not follow the first-order kinetics with a coefficient of determination value of 0.883 and 0.838 for the recommended dose and four times the recommended dose, respectively. The half-life (T 1/2) value of total imidacloprid was observed to be 10.64 and 10.10 days for the recommended dose and four times the recommended dose, respectively.  相似文献   

8.
The present study aimed at evaluating the dissipation of S-metolachlor (S-MET) at three doses in maize growing on diverse physico-chemical properties of soil. The effect of herbicide on dehydrogenase (DHA) and acid phosphatase (ACP) activity was estimated. A modified QuEChERS method using LC-MS/MS has been developed. The limit of quantification (0.001 mg kg?1) and detection (0.0005 mg kg?1) were very low for soil and maize samples. The mean recoveries and RSDs for the six spiked levels (0.001–0.5 mg kg?1) were 91.3 and 5.8%. The biggest differences in concentration of S-MET in maize were observed between the 28th and 63rd days. The dissipation of S-MET in the alkaline soil was the slowest between the 2nd and 7th days, and in the acidic soil between the 5th and 11th days. DT50 of S-MET calculated according to the first-order kinetics model was 11.1–14.7 days (soil) and 9.6–13.9 days (maize). The enzymatic activity of soil was higher in the acidic environment. One observed the significant positive correlation of ACP with pH of soil and contents of potassium and magnesium and negative with contents of phosphorus and organic carbon. The results indicated that at harvest time, the residues of S-MET in maize were well below the safety limit for maize. The findings of this study will foster the research on main parameters influencing the dissipation in maize ecosystems.  相似文献   

9.
Chlorantraniliprole, an anthranilic diamide insecticide with novel mode of action is found effective against several lepidopteran as well as coleopteran, dipteran, and hemipteran pests. The present studies were carried out to study the dissipation pattern of chlorantraniliprole on cauliflower and to suggest suitable waiting period for the safety of consumers. Quick, easy, cheap, effective, rugged, and safe method was used for the extraction and cleanup of samples and the residues of chlorantraniliprole were estimated using high-performance liquid chromatograph (HPLC) and confirmed by liquid chromatograph–mass spectrometer and high-performance thin layer chromatograph. Following three applications of chlorantraniliprole (Coragen 18.5 SC) at recommended dose (9.25 g a.i.?ha?1) and double the recommended dose (18.50 g a.i.?ha?1), the average initial deposits of chlorantraniliprole were observed to be 0.18 and 0.29 mg kg?1, respectively. These deposits were found to be less than the maximum residue limit of 2.0 mg kg?1 prescribed by the Codex Alimentarius Commission. These residues dissipated below the limit of quantification of 0.10 mg kg?1 after 3 and 5 days at recommended and double the recommended dosages, respectively. The half-life value (T 1/2) of chlorantraniliprole was worked out to be 1.36 days following its application at recommended dosages. Hence, the use of this pesticide at recommended dosages does not seem to pose any risk, and a waiting period of 1 day is suggested for safe consumption of cauliflower curds.  相似文献   

10.
A supervised open field trial was conducted to evaluate the dissipation pattern and risk assessment of flubendiamide in gherkin fruits following foliar application of Fame 480 SC at 60 and 120 g a.i.?ha?1. Samples of gherkin fruits were drawn at different time intervals and quantified by HPLC-DAD. The maximum initial deposits of flubendiamide on gherkin were found to be 0.79 and 1.52 mg kg?1, respectively, at recommended and double the recommended doses. The dissipation pattern of flubendiamide followed a first-order kinetics with half-lives of 1.87 to 2.16 days at 60 and 120 g a.i.?ha?1, respectively. The limit of quantification of flubendiamide and desiodo flubendiamide was observed to be 0.01 mg kg?1 for gherkin fruit and soil substrates. Theoretical maximum residue contribution (TMRC) for flubendiamide was calculated and found to be well below the maximum permissible intake (MPI) on gherkin fruits. Thus, the application of flubendiamide at the recommended dose on gherkin fruits presents no human health risks and safe to consumers.  相似文献   

11.
Supervised field trials were conducted at four different agro-climatic locations of India to evaluate the dissipation pattern and risk assessment of spiromesifen on tomato. Spiromesifen 240 SC was sprayed on tomato at 150 and 300 g a.i.?ha?1. Samples of tomato fruits were drawn at 0, 1, 3, 5, 7, 10 and 15 days after treatment and soil at 15 days after treatment. Quantification of residues was done on gas chromatograph–mass spectrophotometer in selective ion monitoring mode in the mass range of 271–274 (m/z). The limit of quantification of the method was found to be 0.05 mg kg?1, while the limit of determination was 0.015 mg kg?1. Residues were found below the LOQ of 0.05 mg kg?1 in 10 days at both the doses of application at all the locations. Spiromesifen dissipated with a half-life of 0.93–1.38 days at the recommended rate of application and 1.04–1.34 days at the double the rate of application. Residues of spiromesifen in soil were detectable level (<0.05 mg kg?1) after 15 days of treatment. A preharvest interval (PHI) of 1 day has been recommended on tomato on the basis of data generated under All India Network Project on Pesticide Residues. Spiromesifen 240 SC has been registered for its use on tomato by Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of spiromesifen on tomato has been fixed by Food Safety Standard Authority of India, Ministry of Health and Family Welfare, Government of India as 0.3 μg/g after its risk assessment.  相似文献   

12.
Proper assessment of soil cadmium (Cd) concentrations is essential to establish legislative limits. The present study aimed to assess background Cd concentrations in soils from the state of São Paulo, Brazil, and to correlate such concentrations with several soil attributes. The topsoil samples (n?=?191) were assessed for total Cd contents and for other metals using the USEPA 3051A method. The background concentration was determined according to the third quartile (75th). Principal component analysis, Spearman correlation, and multiple regressions between Cd contents and other soil attributes (pH, cation exchange capacity (CEC), clay content, sum of bases, organic matter, and total Fe, Al, Zn, and Pb levels) were performed. The mean Cd concentration of all 191 samples was 0.4 mg kg?1, and the background concentration was 0.5 mg kg?1. After the samples were grouped by parent material (rock origin) and soil type, the background Cd content varied, i.e., soils from igneous, metamorphic, and sedimentary rocks harbored 1.5, 0.4, and 0.2 mg kg?1 of Cd, respectively. The background Cd content in Oxisols (0.8 mg kg?1) was higher than in Ultisols (0.3 mg kg?1). Multiple regression demonstrated that Fe was primarily attributed to the natural Cd contents in the soils (R 2?=?0.79). Instead of a single Cd background concentration value representing all São Paulo soils, we propose that the concentrations should be specific for at least Oxisols and Ultisols, which are the primary soil types.  相似文献   

13.
Supervised field trials were conducted at four different agro-climatic zones in India to evaluate the dissipation pattern and risk assessment of flubendiamide on tomato. Flubendiamide 480 SC was sprayed on tomato at 48 and 96 g active ingredient (a.i.) ha?1. Samples of tomato fruits were drawn at 0, 1, 3, 5, 7, 10, 15, and 20 days after treatment. Quantification of residues was done on a high-performance liquid chromatography (HPLC) device with a photo diode array detector. The limit of quantification (LOQ) of this method was found to be 0.01 mg kg?1 while limit of detection (LOD) being 0.003 mg kg?1. Residues of flubendiamide were found below the determination limit of 0.01 mg kg?1 in 20 days at both the dosages in all the locations. The half-life of flubendiamide at an application rate of 48 g a.i.?ha?1 varied from 0.33 to 3.28 days and at 48-g a.i. ranged from 1.21 to 3.00 days. On the basis of data generated under the All India Network Project on Pesticide Residues, a preharvest interval (PHI) of 1 day has been recommended, and the flubendiamide 480 SC has been registered for its use on tomato by the Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of flubendiamide on tomato has been fixed by the Ministry of Health and Family Welfare, Government of India under Food Safety Standard Authority of India, as 0.07 μg g?1 after its risk assessment.  相似文献   

14.
In a preliminary study, we found that the cadmium (Cd) concentrations in shoots of the winter farmland weeds Cardamine hirsuta Linn. and Gnaphalium affine D. Don exceeded the critical value of a Cd-hyperaccumulator (100 mg kg?1), indicating that these two farmland weeds might be Cd-hyperaccumulators. In this study, we grew these species in soil containing various concentrations of Cd to further evaluate their Cd accumulation characteristics. The biomasses of C. hirsuta and G. affine decreased with increasing Cd concentrations in the soil, while the root/shoot ratio and the Cd concentrations in shoot tissues increased. The Cd concentrations in shoots of C. hirsuta and G. affine reached 121.96 and 143.91 mg kg?1, respectively, at the soil Cd concentration of 50 mg kg?1. Both of these concentrations exceeded the critical value of a Cd-hyperaccumulator (100 mg kg?1). The shoot bioconcentration factors of C. hirsuta and G. affine were greater than 1. The translocation factor of C. hirsuta was less than 1 and that of G. affine was greater than 1. These findings indicated that C. hirsuta is a Cd-accumulator and G. affine is Cd-hyperaccumulator. Both plants are distributed widely in the field, and they could be used to remediate Cd-contaminated farmland soil in winter.  相似文献   

15.
Fipronil belongs to phenylpyrazole class of chemical compounds. Degradation of fipronil in sandy loam soil was investigated under field conditions by applying fipronil (Regent 5 % SC) at 50 (T 1) and 100 g a.i. ha?1 (T 2) in field. Samples were drawn periodically in triplicate on 0 (1 h after treatment), 1, 3, 7, 10, 15, 30, 60, and 90 days after treatment and analyzed on GC-ECD system equipped with capillary column. The residues of fipronil in both the doses dissipated in the range of 93.33–100 % in 90 days. Limit of detection (LOD) and limit of determination (LODe/LOQ) were 0.0003 and 0.001 mg kg?1, respectively. Dissipation followed a biphasic first-order kinetics with half-life values of 10.81 and 9.97 days for fipronil alone and 8.14 and 13.05 days for fipronil along with metabolites in soil at (T 1) and (T 2) treatments, respectively.  相似文献   

16.
Metaflumizone is a novel sodium channel blocker insecticide of semicarbazone class. It provides good to excellent control of most of the economically important lepidopterous pests and certain pests in the orders Coleoptera, Hemiptera, Hymenoptera, Diptera, Isoptera, and Siphonaptera. Although metaflumizone has been marketed globally for several years and got registered in India in the year 2009, specifically for the control of DBM on cabbage, to our knowledge, no food safety aspects of metaflumizone residue on cabbage have ever been reported in the literature in India or elsewhere. The present study was undertaken to evaluate the persistence of metaflumizone on cabbage and soil, vis-a-vis its risk assessment, following two spray applications of metaflumizone 220 SC (Verismo®), each at recommended and double dose of 200 and 400 g?a.i.?ha?1 respectively. Initial residue deposits of metaflumizone on cabbage were 0.46 and 0.51 mg?kg?1 at recommended and 0.76 and 0.85 mg?kg?1 at double the recommended dose following the first spray and second spray application. The residues persisted beyond 5 days from both the treatments and dissipated with the half-life ranging from 1.7–2.1 days. Initial deposits of metaflumizone on soil ranged from 0.23–0.37 mg?kg?1 and degraded with a half life ranging from 4.0–4.8 days. No degradation product of metaflumizone was detected in cabbage and soil at any point of time. Soil samples collected from the treated field after 7 days were free from any residue of metaflumizone or its metabolites. A pre-harvest waiting period of 3 days after application was suggested based on calculation of theoretical maximum daily intake.  相似文献   

17.
Metal release from serpentine soils in Sri Lanka   总被引:2,自引:0,他引:2  
Ultramafic rocks and their related soils (i.e., serpentine soils) are non-anthropogenic sources of metal contamination. Elevated concentrations of metals released from these soils into the surrounding areas and groundwater have ecological-, agricultural-, and human health-related consequences. Here we report the geochemistry of four different serpentine soil localities in Sri Lanka by coupling interpretations garnered from physicochemical properties and chemical extractions. Both Ni and Mn demonstrate appreciable release in water from the Ussangoda soils compared to the other three localities, with Ni and Mn metal release increasing with increasing ionic strengths at all sites. Sequential extraction experiments, utilized to identify “elemental pools,” indicate that Mn is mainly associated with oxides/(oxy)hydroxides, whereas Ni and Cr are bound in silicates and spinels. Nickel was the most bioavailable metal compared to Mn and Cr in all four soils, with the highest value observed in the Ussangoda soil at 168?±?6.40 mg kg?1 via the 0.01-M CaCl2 extraction. Although Mn is dominantly bound in oxides/(oxy)hydroxides, Mn is widely dispersed with concentrations reaching as high as 391 mg kg?1 (Yudhaganawa) in the organic fraction and 49 mg kg?1 (Ussangoda) in the exchangeable fraction. Despite Cr being primarily retained in the residual fraction, the second largest pool of Cr was in the organic matter fraction (693 mg kg?1 in the Yudhaganawa soil). Overall, our results support that serpentine soils in Sri Lanka offer a highly labile source of metals to the critical zone.  相似文献   

18.
To understand the residues and ecological risks of veterinary antibiotics (VAs) in animal faeces from concentrated animal feeding operations in northeastern China, 14 VAs were identified by high performance liquid chromatography, and the preliminary risks of six antibiotics were assessed using the hazard quotient (HQ). The investigated VAs occurred in 7.41 to 57.41 % of the 54 samples, and the levels ranged from 0.08 to 56.81 mg kg?1. Tetracyclines were predominant with a maximum level of 56.81 mg kg?1 mostly detected in pig faeces. Sulfonamides were common and detected with the highest concentration of 7.11 mg kg?1. Fluoroquinolones were more widely detected in chicken faeces rather than in pig or cow faeces, which contained the dominant antibiotic enrofloxacin. In comparison, the residue of tylosin was less frequently found. The risk evaluations of the six antibiotics revealed that tetracyclines, especially oxytetracycline, displayed the greatest ecological risk because of its high HQ value of 15.75. The results of this study imply that multiple kinds of VAs were jointly used in animal feeding processes in the study area. These medicine residues in animal faeces may potentially bring ecological risks if the animal manure is not treated effectively.  相似文献   

19.
Top predators like the Neotropical otter, Lontra longicaudis annectens, are usually considered good bioindicators of habitat quality. In this study, we evaluated heavy metal contamination (Hgtot, Pb, Cd) in the riverine habitat, prey (crustaceans and fish), and otter feces in two Ramsar wetlands with contrasting upstream contamination discharges: Río Blanco and Río Caño Grande in Veracruz, Mexico, during the dry, the wet, and the nortes seasons. Most comparisons revealed no differences between sites while seasonal differences were repeatedly detected for all of the compartments. Higher concentrations of Pb during the dry season and of Cd during the wet season in otter feces mirrored differences detected in the most seasonally consumed prey. Compared with fecal methylmercury values reported for the European otter (0.25–0.75 mg kg?1) in unprotected areas, the Hgtot levels that we measured were lower (0.02–0.17 mg kg?1). However, Pb (117.87 mg kg?1) and Cd (9.14 mg kg?1) concentrations were higher (Pb, 38.15 mg kg?1 and Cd, 4.72 mg kg?1) in the two Ramsar wetlands. Protected areas may shelter species, but those with water-linked diets may suffer the effect of chemicals used upstream.  相似文献   

20.
This study investigates adsorption-desorption and the leaching potential of glyphosate and aminomethylphosphonic acid (AMPA) in control and amended—addition of cow dung or rice husk ash—acidic Malaysian soil with high oxide mineral content. The addition of cow dung or rice husk ash increased the adsorptive removal of AMPA. The isotherm data of glyphosate and AMPA best fitted the Freundlich model. The constant Kf for glyphosate was high in the control soil (544.873 mg g?1) followed by soil with cow dung (482.451 mg g?1) then soil with rice husk ash (418.539 mg g?1). However, for AMPA, soil with cow dung was high (166.636 mg g?1) followed by soil with rice husk ash (137.570 mg g?1) then the control soil (48.446 mg g?1). The 1/n values for both glyphosate and AMPA adsorptions were <?1 indicating their strong affinity for adsorbents. Desorption of both glyphosate and AMPA occurred only in the control soil. The compounds were not detected in soils with added cow dung or rice husk ash. The addition of cow dung or rice husk ash increased glyphosate mobility. However, ground water ubiquity scores for both control and amended soils were <?2.8. This indicated glyphosate is a transitional herbicide; therefore, its leaching potential in the soil is low, despite the addition of cow dung or rice husk ash. Addition of these wastes decreased the mobility and leaching potential of AMPA. The addition of cow dung or rice husk ash could be beneficial in increasing adsorption and enhancing degradation of these compounds.  相似文献   

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