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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.
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   

4.
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   

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 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   

6.
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   

7.
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   

8.
A new method has been developed to determine heptachlor and its metabolites heptachlor-exo-epoxide and heptachlor-endo-epoxide in pork. The pork samples were extracted with acetone–n-hexane (2:8, V:V) and cleaned up by gel permeation chromatography and florisil solid-phase extraction cartridge. The extract was then determined by gas chromatography equipped with electron capture detector (GC-ECD), followed by validation using gas chromatography–mass spectrometry (GC–MS) with negative chemical ionization. Linearity of calibration curves ranged from 0.01 to 0.5 mg L?1, with correlation coefficients of more than 0.9980 for GC-ECD and GC–MS, respectively. At spiked concentrations of 0.01, 0.05, and 0.1 mg kg?1, the average recovery and relative standard deviation values were 87.1–102.2 and 4.0–11.3 %, respectively. The limit of quantification for each analyte was 0.01 mg kg?1, which satisfied the current maximum residue limit permitted in pork. Our results showed that the method developed was successfully used to determine heptachlor and heptachlor epoxide residues in real pork samples.  相似文献   

9.
An integrated method for the simultaneous determination of insecticide fipronil and its three metabolites, desulfinyl, sulfide, and sulfone, in maize grain, maize stem, and soil was developed. This three-step method uses liquid–solid extraction with ultrasound or mechanical grinding, followed by liquid–liquid partitioning and florisil solid-phase extraction (SPE) for cleanup. The quantification was conducted by gas chromatography–electron capture detection in triplicate for each sample. The method was validated with five replicates at three fortification concentrations, 0.002, 0.01, and 0.1 mg kg?1, in each matrix and gave mean recoveries from 83 to 106 % with relative standard deviation ≤8.9 %. The limits of quantification (LOQ) were 0.002 mg kg?1 for the compounds in all matrixes. In the field study in Beijing and Shandong 2012, fipronil-coated maize seeds were planted and the proposed method was applied for checking the possible existence of four compounds in maize and soil samples, but none of them contained residues higher than the LOQs in both application rates. Moreover, the dissipation of fipronil in soil fits first-order kinetics with half-lives 9.90 and 10.34 days in Beijing and Shandong, respectively. Combined with an adequate sample treatment, this technique offers good sensitivity and selectivity in the three complex matrixes. The results could provide guidance for the further research on pesticide distribution and safe use of fipronil as seed coat in cereals.  相似文献   

10.
Supervised field trials following good agricultural practices were conducted at the research farms of four agricultural universities located at four different agroclimatic zones of India to evaluate the persistence and dissipation of flubendiamide and its metabolite, des-iodo flubendiamide, on cabbage. Two spray applications of flubendiamide 480 SC of standard and double dose at the rate of 24 and 48 g a.i. ha?1 were given to the crop at a 15-day interval, and the residues of flubendiamide 2 h after spray were found in the range of 0.107–0.33 and 0.20–0.49 mg kg?1 at respective doses. Residue of des-iodo flubendiamide was not detected in any cabbage sample during study period. No residues were found in the soil samples collected from all treated fields after 15 days of application. On the basis of data generated under All India Network Project on Pesticide Residues, a preharvest interval (PHI) of 10 days has been recommended, and the flubendiamide 480 SC has been registered for its use on cabbage by Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of flubendiamide on cabbage has been fixed by the Ministry of Health and Family Welfare, Government of India, under Food Safety Standard Authority of India as 0.05 μg/g after its risk assessment.  相似文献   

11.
The Fusaro Lagoon is a shallow lagoon, located in SW Italy, largely influenced in the last decades by several anthropic impacts. The study examined the pollution status of the lagoon, during year 2011–2012 at nine sampling stations with the aim to find out proper measurements of water lagoon restoration. Concentrations of heavy metals (HMs) (aluminium [Al], barium [Ba], cadmium [Cd], copper [Cu], iron [Fe], manganese [Mn], vanadium [V] and zinc [Zn]) were examined in water, sediments and specimens of the ascidian Ciona intestinalis sp. A. Low levels of dissolved oxygen concentration were detected at many stations, with mean values of 5.2–6.4 mg L?1. The redox potential of surface waters was also low, ?2.7 to 50.7 mV. Sediments possessed high organic matter content, 17.7–29.4 %. In sediments, the mean Zn level, 251.4 mg kg?1, was about sixfold higher than that recorded in year 2000 (38.5 mg kg?1) and considerably higher than that recorded in 2007 (191 mg kg?1). The mean levels of Cd were outstandingly high, with a mean value of 70.5 mg kg?1, about 30- and 50-fold higher than those determined in 2000 and 2007, respectively. Cadmium (Cd), Cu and nickel (Ni) appeared in excess with respect to most current guidelines, reaching significant pollution levels. C. intestinalis sp. A was detected only at few stations, with metals accumulated preferentially in the body in respect to the tunic, from 1.2 times for Zn (178 mg kg?1) to 4.0 times for V (304 mg kg?1). Data suggests the necessity of an immediate action of eco-compatible interventions for environmental restoration.  相似文献   

12.
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   

13.
Dissipation and decontamination of the semisynthetic macrolide emamectin benzoate and the natural insecticide spinosad on cowpea pods were studied following field application at single and double doses of 11.0 and 22 and 73 and 146 g ai ha?1, respectively. Residues of these naturalytes were estimated using LC-MS/MS. The initial deposit of 0.073 and 0.153 mg kg?1 of emamectin benzoate dissipated below quantitation level on the fifth and seventh day at single and double dosage, respectively. For spinosad, the initial deposits of 0.94 and 1.90 mg kg?1 reached below quantitation level on the 7th day and 15th day at single and double dosage, respectively. The half-life of emamectin benzoate and spinosad was 1.13–1.49 and 1.05–1.39 days with the calculated safe waiting period of 2.99–6.12 and 1.09–3.25 days, respectively, for single and double dosage. Processing of the harvestable pods with different decontamination techniques resulted in 33.82 to 100 % removal 2 h after the application of emamectin benzoate and 100 % removal 3 days after spraying, while the removal was 42.05 to 87.46 % 2 h after the application of spinosad and 38.05 to 68.08 % 3 days after application.  相似文献   

14.
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   

15.
Quizalofop ethyl, a phenoxy propionate herbicide, is used for postemergence control of annual and perennial grass weeds in broad-leaved crops in India. The experiments were designed to study the dissipation kinetics of quizalofop ethyl on onion for two seasons. A simple, rapid, and sensitive method for estimation of quizalofop ethyl residues in onion and soil was developed and validated. The recoveries of quizalofop ethyl residues from onion and soil at different spiking level range from 84.81 to 92.68 %. The limit of quantification of this method was found to be 0.01 μg g?1. The risk assessment through consumption of the onion in comparison to its acceptable daily intake which is an important parameter for the safety of the consumer was also evaluated. Standardized methodology supported by recovery studies was adopted to estimate residues of quizalofop ethyl on onion and soil. The average initial deposits of quizalofop ethyl on onion were observed to be 0.25 and 0.33 mg kg?1, following single application of the herbicide at 50 g active ingredient (a.i.) ha?1 during 2009 and 2010, respectively. The half-life values (T 1/2) of quizalofop ethyl on onion crop were worked out to be 0.85 and 0.79 days, respectively, during 2009 and 2010. At harvest time, the residues of quizalofop ethyl on onion and soil were found to be below the determination limit of 0.01 mg kg?1 following single application of the herbicide at 50 and 100 g a.i. ha?1 for both the periods.  相似文献   

16.
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   

17.
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   

18.
Located in Central South China, Hunan province is rich in mineral resources. To study the influence of mining on Cd pollution to local agricultural eco-system, the paddy soils and rice grain of Y county in northern Hunan province were intensively monitored. The results were as follows: (1) Total Cd (T-Cd) content in the soils of the county ranges from 0.13 to 6.02 mg kg?1, with a mean of 0.64 mg kg?1, of which 57.5 % exceed the allowable limit specified by the China Soil Environmental Quality Standards. T-Cd in the soils varies largely, with the coefficient of variation reaching 146.4 %. The spatial distribution of T-Cd in the soils quite matches with that of mining and industries. The content of HCl-extractable Cd (HCl-Cd) in the soils ranges from 0.02 to 2.17 mg kg?1, with a mean of 0.24 mg kg?1. A significant positive correlation exists between T-Cd and HCl-Cd in the soils (r?=?0.770, ρ?<?0.01). (2) Cd content in the rice produced in Y county ranges from 0.01 to 2.77 mg kg?1, with a mean of 0.46 mg kg?1. The rate of rice with Cd exceeding the allowable limit specified by the Chinese Grain Security Standards reaches 59.6 %; that with Cd exceeding 1 mg kg?1, called as “Cd rice,” reaches 11.1 %. (3) Cd content in the rice of Y county is positively significantly correlated with HCl-Cd (r?=?0.177, ρ?<?0.05) but not significantly with T-Cd in the soils (r?=?0.091, ρ?>?0.05), which suggests that the amount of Cd accumulating in the rice is more affected by its availability in the soils, rather than the total content. (4) The dietary intake of Cd via rice consumption in Y county is estimated to be 179.9 μg day?1 person?1 on average, which is far beyond the allowable limit specified by FAO/WHO and the target hazard quotients of Cd much higher than 1, suggesting the high risk on human health from Cd exposure.  相似文献   

19.
Food safety is a global concern due to the increased use of pesticides in agriculture. In grapes, carbendazim is one of the frequently detected fungicides. However, it is amenable to biodegradation. In this study, we aimed to assess the degradation of carbendazim by four Bacillus subtilis strains, which had earlier shown potential for biocontrol of grape diseases. In liquid medium, each of the four strains, namely, DR-39, CS-126, TL-171, and TS-204, could utilize carbendazim as the sole carbon source. The half-life was minimized from 8.4 days in the uninoculated spiked control to 4.0–6.2 days by the four strains. In Thompson Seedless sprayed with carbendazim at 1.0 g L?1, the residue on grape berries in control was 0.44 mg kg?1 after 25 days of application, whereas in grapes treated with the four B. subtilis strains, the residues had decreased to 0.02 mg kg?1. The degradation kinetics showed low half-lives of 3.1 to 5.2 days in treated grapes as compared to 8.8 days in control. In inoculated soils, the half-lives were 5.9 to 7.6 days in autoclaved and 6.5 to 7.2 days in nonautoclaved soils as compared to 8.2 and 8.0 days in respective controls. The growth dynamics of these strains in all the three matrices was not affected by presence of carbendazim. Bacillus strains TS-204 and TL-171 showed higher degradation rate than the other two strains in all the three matrices and show promise for in situ biodegradation of carbendazim.  相似文献   

20.
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   

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