Dissipation, residues, and risk assessment of spirodiclofen in citrus

The dissipation, residues, and distribution of spirodiclofen, a new type of insecticide and acaricide that belongs to the class of ketoenols or tetronic acids, in citrus were investigated in this study. Risk assessment of sprodiclofen was also conducted based on those data. The open-field experiments were conducted in Guangdong, Fujian, and Guangxi of China. Results showed that the half-lives in citrus ranged from 6.5 to 13.6 days at three sites. The terminal residues of spirodiclofen were all below the FAO/WHO maximum residue limit of 0.5 mg/kg in citrus, when they were determined 14 days after final application. Distribution of spirodiclofen in peel and flesh was analyzed, and residues were found to be concentrated on peel. Risk assessment was performed by calculation of risk quotient, which showed that the use of spirodiclofen is comparably safe for humans.     

Dissipation and residue of 2,4-<Emphasis Type="SmallCaps">d</Emphasis> in citrus under field condition

The dissipation, residues, and risks of 2,4-dicholrophenoxyacetic acid (2,4-d) in citrus under field condition were investigated based on a simple ultra-performance LC (UPLC)-MS/MS method. The results indicated that the residue level of 2,4-d in citrus did not degrade gradually with sampling time under field condition. At pre-harvest intervals (PHI) of 20–40 days, 2,4-d residues were 0.021–0.269 mg/kg in citrus flesh, 0.028–0.337 mg/kg in whole citrus, and 0.028–0.376 mg/kg in citrus peel, all bellow the China maximum residue limit in citrus (1 mg/kg). Risks of 2,4-d were assessed by calculation of risk quotient, and the results revealed no significant health risks after consumption of citrus.     

Dissipation pattern and risk quotients assessment of amisulbrom in Korean melon cultivated in plastic house conditions

Amisulbrom formulated as suspension concentrate was applied at the rate recommended for Korean melon to determine the dissipation pattern (at two different sites), the pre-harvest residue limit (PHRL), and risk assessments. Samples collected over 10 days were extracted using liquid-liquid extraction (LLE) and cleaned up with solid-phase extraction (SPE) Florisil cartridge. Residual concentrations were determined using liquid chromatography-ultraviolet detector (LC-UVD) and confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard showed good instrument response linearity with a correlation coefficient (R ²) = 0.9999, and the recovery ranged from 87.5 to 93.7%. The dissipation half-life calculated from two different sites were found to be 7.0 and 8.8 days for sites 1 and 2, respectively. A PHRL graph constructed from the data indicated that if the residue levels were less than 0.55–0.59 mg/kg 3 days before harvest or less than 0.61–0.74 mg/kg 7 days before harvest, then they would be lower than the maximum residue limits (MRLs) at harvest. Risk assessments showed that the risk quotient (RQ) was 4.39–3.47% at 0 day, declined to 1.53–1.63% at 10 days. Therefore, the current data indicate that the amisulbrom can be applied safely to Korean melon; hence, it is unlikely to induce adverse health effects in consumers.     

Dissipation and residues determination of propamocarb in ginseng and soil by high-performance liquid chromatography coupled with tandem mass spectrometry

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.     

Persistence and dissipation of flubendiamide and its risk assessment on gherkin (Cucumis anguria L.)

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.     

Residues and dissipation of trifloxystrobin and its metabolite in tomatoes and soil

A simple residue analytical method using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure for the determination of trifloxystrobin and its metabolite trifloxystrobin acid (CGA321113) in tomato and soil was developed using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The limits of detection were 0.0005 mg/kg for trifloxystrobin and 0.001 mg/kg for trifloxystrobin acid, respectively. The average recoveries in tomato and soil ranged from 73–99 % for trifloxystrobin and 75–109 % for trifloxystrobin acid, with relative standard deviations below 15 %. The method was then used to study the dissipation and residues in tomato and soil. The dissipation half-lives of trifloxystrobin in tomato were 2.9 days (Beijing) and 5.4 days (Shandong), while in soil were 1.9 days (Beijing) and 3.0 days (Shandong), respectively. The final results showed that the major residue compound was trifloxystrobin in tomato whereas it was its metabolite, trifloxystrobin acid, in soil. The final residues of total trifloxystrobin (including trifloxystrobin acid) were below the EU maximum residue limit of 0.5 mg kg^?1 in tomato 3 days after the treatment.     

Dissipation and residue of azoxystrobin in banana under field condition

A method was developed for determining azoxystrobin in banana and cultivation soil using gas chromatography. The dissipation and residue of azoxystrobin in banana fields at GAP conditions were investigated. The average recoveries ranged from 80.3 to 96.0 % with relative standard deviations of 2.9 to 7.2 % at three different spiking levels for each matrix. The results indicated that the half-life of azoxystrobin in bananas and soil ranged from 7.5 to 13.5 days in Guangdong and from 8.7 to 12.7 days in Fujian. The dissipation rates of azoxystrobin in banana and soil were almost the same. Terminal residues in banana and banana flesh (0.01 mg/kg) were all below the maximum residue limit (2 mg/kg by Codex Alimentarius Commission and China). The results demonstrated that the safety of using azoxystrobin at the recommended agriculture dosage to protect bananas from diseases.     

Dissipation and residue of triforine in strawberry and soil

Two independent field trials were performed in Guangdong and Hubei, China in 2011 to investigate the dissipation and residue levels of triforine in strawberry and soil. A fast and simple method using gas chromatography with electron capture detector was developed and validated to determine triforine levels in strawberry and soil. The average recovery of triforine in strawberry ranged from 87.46 to 104.32 % with a relative standard deviation (RSD) of 0.72 to 4.54 %; that in soil ranged from 83.82 to 103.01 % with an RSD of 3.89 to 4.36 %. The limit of quantification of the proposed method was 0.01 mg/kg for both strawberry and soil. The results suggest that the triforine dissipation curves followed the first-order kinetic. The half-lives of triforine in strawberry from Guangdong and Hubei were 3.58 and 4.42 days, respectively; those in soil were 3.53 and 4.10 days, respectively. The terminal residues of triforine in strawberry ranged from 0.032 to 0.264 mg/kg at preharvest intervals of 0.5, 1, and 3 days. These values are lower than the maximum residue limit of 1 mg/kg in strawberry set by the Codex Alimentarius Commission.     

Persistence and risk assessment of spiromesifen on tomato in India: a multilocational study

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.     

Dissipation and residue behavior of mepiquat on wheat and potato field application

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.     

Dissipation and residues of bispyribac-sodium in rice and environment

The dissipation and residues of bispyribac-sodium in rice cropping system were studied. Bispyribac-sodium residues were extracted by a simple analytical method based on QuEChERs and detected by LC-MS/MS. The limit of detection for bispyribac-sodium of this method was 0.375?×?10^?3 ng. The limit of quantification (LOQ) was 5.0 μg/kg for rice plant samples, 2.0 μg/kg for rice hull, 0.2 μg/kg for water, and 0.1 μg/kg for soil and husked rice samples. The average recoveries of bispyribac-sodium ranged from 74.7 to 108 %, with relative standard deviations less than 13 %. The half-lives of bispyribac-sodium in rice plant, water, and soil were in the range of 1.4–5.6 days. More than 90 % of bispyribac-sodium residue dissipated within 5 days. The final residues of bispyribac-sodium in rice were all below LOQ at harvest time.     

Dissipation of S-metolachlor in plant and soil and effect on enzymatic activities

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.     

Evaluation of environmental fate of acetamiprid in the laboratory

The acetamiprid, a nenicotinoid insecticide, is a popular crop protection agent used in fields as well as in protected cultivation. A laboratory experiment was conditions to study the effect of light, moisture, and pH on the persistence of acetamiprid in water and soil. Dissipation half-lives of acetamiprid in water at pH 4, 7, and 9 were 6.2, 7.3, and 5.1 days, respectively, and 4.3 days under UV and sunlight conditions. Half-life in soil at three concentrations, 0.1, 1.0, and 10 μg g^?1 under different moisture regimes varied from 21.5–22.8, 15.6–22.4, 10.0–15.8 days, respectively, indicating that acetamiprid dissipated faster in submerged soil as compared to field capacity moisture and dry conditions. The leaching study showed that the possibility for leaching of acetamiprid to ground water is extremely low under normal condition of average rainfall due to compact nature soil in the field. Acetamiprid poses low risks to the ecosystem because of their rapid dissipation and low-bound residues in the environment.     

Persistence of metaflumizone on cabbage (Brassica oleracea Linne) and soil, and its risk assessment

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.     

Persistence and effect of processing on reduction of chlorantraniliprole residues on brinjal and okra fruits

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.     

Dissipation and residue of metalaxyl and cymoxanil in pepper and soil

A simple and accurate method of determining metalaxyl and cymoxanil in pepper and soil was developed by ultra-performance liquid chromatography–photodiode array detection. The limits of detection were 0.015 mg/kg for metalaxyl and 0.003 mg/kg for cymoxanil. The limits of quantification were 0.05 mg/kg for metalaxyl in pepper and soil as well as 0.01 mg/kg for cymoxanil in pepper and soil. Recoveries of pepper and soil were investigated at three spiking levels and ranged within 77.52 to 102.05 % for metalaxyl and 87.15 to 103.21 % for cymoxanil, with relative standard deviations below 9.30 %. For field experiments, the half-lives of metalaxyl were 3.2 to 3.9 days in pepper and 4.4 to 9.5 days in soil at the three experimental locations in China. At harvest, pepper samples were found to contain metalaxyl and cymoxanil well below the maximum residue limit MRLs of the European Union (EU) following the recommended dosage and the interval of 21 days after last application.     

Safety evaluation of flubendiamide and its metabolites on cabbage and persistence in soil in different agroclimatic zones of India

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.     

Dissipation kinetics of tetraconazole in three types of soil and water under laboratory condition

Laboratory experiment was conducted to understand the persistence behavior of tetraconazole in three soils of West Bengal (alluvial, red lateritic, and coastal saline) and also in water maintained at three different pH (4.0, 7.0, and 9.2) conditions. Processed soil samples (100 g) were spiked at two treatment doses: 2.5 μg/g (T₁) and 5.0 μg/g (T₂). Double distilled buffered water (200 ml) was spiked at two treatment doses: 1.0 μg/ml (T₁) and 2.00 μg/ml (T₂). The tetraconazole dissipation followed first-order reaction kinetics and the residual half-life (T _1/2) values in soil were found to be in the range of 66.9–77.2 days for T₁ and 73.4–86.0 days for T₂. The persistence increased in the order red lateritic > new alluvial > coastal saline. Interestingly, the red lateritic soil exhibited the lowest pH (5.56) and organic carbon (0.52 %) content as compared to other two soils. However, the dissipation of tetraconazole in case of water was not pH dependant. The T _1/2 values in water were in the range of 94 to 125 days. The study indicated the persistent nature of tetraconazole in soil and water.     

Dissipation and residue of famoxadone in grape and soil

The analytical method of famoxadone residue and its dissipation in grape and soil were investigated. Famoxadone (68.75% water-dispersible granule) was applied at two dosages (1.25 and 2.5 g l^???1). Soil and grape samples were collected at intervals and analyzed for famoxadone residues. The results showed that the degradation rate of famoxadone in grape and soil were similar, and their dynamics could be described by C?=?1.1738e ^???0.0562t with correlation coefficient r?=?0.9044 in grape and C?=?5.6565e ^???0.0515t with r?=?0.9620 in soil, respectively. Half-lives were 12.3 and 13.5 days in grape and soil, respectively. The results indicated that at harvest time, the residues of famoxadone in grape were well below the EU’s maximum residue level (2 mg kg^???1) and was safe to apply in grape.     

Dissipation kinetics and residues of triazolopyrimidine herbicides flumetsulam and florasulam in corn ecosystem

The dynamic and residues of florasulam and flumetsulam in corn field ecosystem were investigated using quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The limits of quantification (LOQs) of the proposed method ranged from 0.005 to 0.01 mg/kg. Mean recoveries and relative standard deviations (RSDs) of the two compounds in all samples at three spiking levels ranged 94–110 % and 2.0–9.2 %, respectively. Florasulam and flumetsulam degradation followed first-order kinetics with half-lives 1.7–2.9 and 3.3–8.7 days in soil and 1.3–1.8 and 0.9–1.7 days in plant, respectively. The residues in all the samples were found to be less than the LOQs at preharvest intervals of 53 and 78 days. The results suggest that the combined use of florasulam and flumetsulam on corn is considered to be safe under the recommended conditions and can be utilized for establishing the maximum residue limit (MRL) of florasulam in corn in China.