Dissipation kinetics and consumer risk assessment of novaluron + lambda-cyhalothrin co-formulation in cabbage.

Cabbage, one of the most popular vegetables in the world is infested by several insect-pests and diseases. Novaluron, a chitin synthesis inhibitor and lambda-cyhalothrin, a synthetic pyrethroid group insecticide are used to manage insect-pests on cabbage. The dissipation kinetics and risk assessment of combination formulation (novaluron 9.45% + lambda-cyhalothrin 1.9%) with different modes of action has not yet been investigated in cabbage. Multi-location supervised field trials were therefore, conducted in different agro-climatic regions of India for safety evaluation of the combination product. The co-formulation at the recommended (novaluron 750 g a.i. ha-1 + lambda-cyhalothrin 750 g a.i. ha-1) and double the recommended (novaluron 1500 g a.i. ha-1 + lambda-cyhalothrin 1500 g a.i. ha-1) dose was sprayed on the cabbage crop. The samples were extracted and cleaned up using a modified QuEChERS method, and the residues analyzed by GC-ECD and GC-MS. The half-life (t1/2) varied between 1.77 and 2.51 and 2.00-3.38 days for novaluron and 1.36-2.24 and 1.69-3.82 days for lambda-cyhalothrin in cabbage at respective doses. The Food Safety and Standards Authority of India (FSSAI) has set the MRL of 0.7 mg kg-1 for novaluron at PHI of 5 days, and no MRL is set for lambda-cyhalothrin in cabbage. On the basis of OECD MRL calculator, the MRLs of 0.6 and 1.5 mg kg-1 for novaluron and lambda-cyhalothrin, respectively were calculated at the respective doses at PHI of 3 days. Hazard quotient (HQ) <1, theoretical maximum daily intake (TMDI) < acceptable daily intake (ADI) and < maximum permissible intake (MPI), percent acute hazard index (% aHI) <1, and percent chronic hazard index (% cHI) <1 for both novaluron and lambda-cyhalothrin suggested that the combination formulation is safe and will not pose any dietary risk to the consumers. The study will be helpful to conduct risk assessment of other pesticides/combination pesticides on food crops on which their MRLs have not yet been fixed.

Dissipation of neonicotinoid insecticides imidacloprid, indoxacarb and thiamethoxam on pomegranate (Punica granatum L.).

Neonicotinoid insecticides such as imidacloprid, indoxacarb and thiamethoxam are widely used for control of a large number of insect pests of pomegranate crop. Their residue levels were evaluated on pomegranate fruits over 2 years during the same cropping season. The QuEChERS analytical method in conjunction with LC-MS/MS was validated to analyse the insecticides on pomegranate fruits with peel (whole fruit), without peel (aril) and in the field soil. The method performance was satisfactory with the limit of quantification (LOQ) of 0.005 mg/kg which was below the maximum residue limits (MRLs) in pomegranate for the 3 compounds. A first order reaction kinetics was observed for the three insecticides with the half -life of degradation of 8-11.1 days for imidacloprid; 7.4-8.4 days for indoxacarb and 9.8-14.2 days for thiamethoxam. Though the insecticides are systemic in nature, the residues in the edible pomegranate aril were always < LOQ. The maximum residue levels of imidacloprid on pomegranate was less than its MRL of 1 mg/kg, so the pre-harvest interval (PHI) required was 1 day only. For indoxacarb, 31-42 days PHI was needed for the residues to reduce to its MRL of 0.02 mg/kg. The PHI of thiamethoxam was 46-77 days, the time required for its residues to reduce to its MRL of 0.01 mg/kg. Higher rainfall possibly facilitated faster dissipation of imidacloprid residues from pomegranate whereas indoxacarb and thiamethoxam remained unaffected. The results of the study can be utilized to incorporate these three chemicals in the plant protection program of pomegranate and fixation of MRL in India.

Dissipation pattern of flubendiamide residues on capsicum fruit (Capsicum annuum L.) under field and controlled environmental conditions.

This investigation was undertaken to compare the dissipation pattern of flubendiamide in capsicum fruits under poly-house and open field after giving spray applications at the recommended and double doses of 48 g a.i. ha(-1) and 96 g a.i. ha(-1). Extraction and purification of capsicum fruit samples were carried out by the QuEChERS method. Residues of flubendiamide and its metabolite, des-iodo flubendiamide, were analyzed by high-performance liquid chromatography-photodiode array, and confirmed by liquid chromatography-mass spectrometry/mass spectrometry. Limit of quantification of the method was 0.05 mg kg(-1), and recovery of the insecticides was in the range of 89.6-104.3%, with relative standard deviation being 4.5-11.5%. The measurement uncertainty of the analytical method was in the range of 10.7-15.7%. Initial residue deposits of flubendiamide on capsicum fruits grown under poly-house conditions were (0.977 and 1.834 mg kg(-1)) higher than that grown in the field (0.665 and 1.545 mg kg(-1)). Flubendiamide residues persisted for 15 days in field-grown and for 25 days in poly-house-grown capsicum fruits. The residues were degraded with the half-lives of 4.3-4.7 and 5.6-6.6 days in field and poly-house respectively. Des-iodo flubendiamide was not detected in capsicum fruits or soil. The residues of flubendiamide degraded to below the maximum residue limit notified by Codex Alimentarius Commission (FAO/WHO) after 1 and 6 days in open field, and 3 and 10 days in poly-house. The results of the study indicated that flubendiamide applied to capsicum under controlled environmental conditions required longer pre-harvest interval to allow its residues to dissipate to the safe level.

Residue level and dissipation of carbendazim in/on pomegranate fruits and soil.

Carbendazim is widely used on pomegranate for control of a large number of fungal diseases. Its residue levels in/on pomegranate fruits and soil were evaluated under field conditions. The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method in conjunction with liquid-chromatography mass spectrometry was used for analysis of carbendazim. Recovery of carbendazim was within 78.92-96.28 % and relative standard deviation within 3.8-10.9 % (n = 6). Carbendazim residues on pomegranate fruits dissipated at the half lives of 17.3 and 22.8 days from treatments at 500 and 1000 g active ingredient (a.i.) ha(-1), respectively. Its residues in pomegranate aril were highest on the tenth day and reduced thereafter. The residue level of carbendazim on pomegranate whole fruits from standard dose treatment was less than the EU maximum residue limit (MRL) of 0.1 mg kg(-1) at harvest. The carbendazim residues were

Residue level and dissipation pattern of spiromesifen in cabbage and soil from 2-year field study.

Spiromesifen is a new class of insecticide used for the control of whiteflies and mites which have developed resistance to the more commonly used neonicotinoids. Dissipation pattern of spiromesifen on cabbage was evaluated over 2 years by conducting supervised field studies as per good agricultural practices. Cabbage and soil samples were extracted and purified using modified QuEChERS method and analyzed through gas chromatography (GC). Confirmatory studies were carried out by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The recoveries of spiromesifen from cabbage and soil were between 85.44 and 103.37% with the relative standard deviation (RSD) between 3.2 and 9.4% (n = 6). The limit of detection (LOD) and limit of quantification (LOQ) were 0.003 µg mL(-1) and 0.01 mg kg(-1), respectively. The measurement uncertainties (MUs) were within 9.9-14.9%. Initial residues of spiromesifen on cabbage were 0.640 and 1.549 mg kg(-1) during 2013 and 0.723 and 1.438 mg kg(-1) during 2014 from treatments at standard and double doses of 125 and 250 g active ingredient (a.i.) ha(-1), respectively. Spiromesifen residue dissipation followed first-order rate kinetics, and it degraded within the half-lives of 2.9 and 3.9 days during 2013 and 3.2 and 4.5 days during 2014. The residue levels reached below the maximum residue limit (MRL; 0.02 mg kg(-1)) within 15-17 days at the standard dose and 24-27 days at the double dose. The field soil analyzed at harvest (30 days) was free from spiromesifen residues. Metabolite spiromesifen-enol was not detected in any sample which was confirmed through LC-MS/MS analysis.

Comparison of the residue persistence of trifloxystrobin (25%) + tebuconazole (50%) on gherkin and soil at two locations.

Residue study of trifloxystrobin and tebuconazole on gherkin was carried out at two locations (Bangalore and Gouribiddunur, India) after applications at the standard and double doses of 75 + 150 and of 150 + 300 g ha(-1) of the formulated product, trifloxystrobin (25%) + tebuconazole (50%) (Nativo 75 WG). The fungicides were determined by gas chromatography (GC) and confirmed by gas chromatography-mass spectrometry (GC-MS). Extraction and purification of the samples were carried out by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method after validating the analytical parameters. Initial residues of trifloxystrobin on gherkin fruits were 0.335 and 0.65 mg kg(-1) at Bangalore, and 0.34 and 0.615 mg kg(-1) at Gouribiddunur. Tebuconazole residues were 0.842 and 1.682 mg kg(-1) at Bangalore, and 0.71 and 1.34 mg kg(-1) at Gouribiddunur. Residue dissipation of the fungicides followed first-order rate kinetics. Trifloxystrobin residues dissipated at the half-life of 2.9-3.7 days, and tebuconazole at 3.2 days. At the standard dose treatment, trifloxystrobin residues dissipated to below the maximum residue limit (MRL) of 0.2 mg kg(-1) (European Union) within 3 days at both the locations. Residues of the metabolite CGA 321113 was less than the limit of quantification (LOQ; 0.05 mg kg(-1)) on all sampling days. Tebuconazole residues dissipated to below its MRL (0.05 mg kg(-1)) within 14 and 11 days, at Bangalore and Gouribiddunur, respectively. From the two trials, it was concluded that the required pre-harvest interval (PHI) for the combination formulation was 14 days. Application of Nativo 75 WG should be given before flowering to allow the residues to dissipate below the MRLs at harvest.

Residue levels and dissipation behaviors for trifloxystrobin and tebuconazole in mango fruit and soil.

An evaluation of residue levels of trifloxystrobin and tebuconazole was carried out on mango fruits after treatments with the combined formulation, trifloxystrobin (25 % w/w) and tebuconazole (50 % w/w), at standard and double doses of 250 + 500 and 500 + 1000 g a.i. ha(-1), respectively. Extraction and purification of the mango fruit samples were carried out by the QuEChERS method after validating the analytical parameters. Determination of the fungicides was carried out by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). The limits of detection (LOD) and limits of quantification (LOQ) for both fungicides were 0.015 µg mL(-1) and 0.05 mg kg(-1), respectively. The residue levels of trifloxystrobin for standard and double-dose treatments were 0.492 and 0.901 mg kg(-1) and for tebuconazole were 0.535 and 1.124 mg kg(-1), respectively. A faster dissipation of tebuconazole in mango fruit was observed compared with that for tebuconazole. Dissipation of trifloxystrobin and tebuconazole in mango followed first-order kinetics, and the half-lives were 9 and 6 days, respectively. The preharvest intervals (PHI), the time taken for the combined residues of trifloxystrobin and tebuconazole to dissipate to their permissible levels (maximum residue limits), were 14 and 20 days for standard and double doses, respectively. At harvest, mature mango fruit and soil were free from fungicide residues.

Residue evaluation of imidacloprid, spirotetramat, and spirotetramat-enol in/on grapes (Vitis vinifera L.) and soil.

A combination of imidacloprid and spirotetramat effectively controls sucking pests on grapevines. Residues of these insecticides on grapes were evaluated after treatment with spirotetramat 12% + imidacloprid 12% (240 SC) three times at 90 and 180 g a.i. ha(-1). The samples were extracted and purified by QuEChERS method and analyzed by high-performance liquid chromatography with a photodiode array detector (imidacloprid) and gas chromatography mass spectrometry (spirotetramat and its metabolite spirotetramat-enol). Satisfactory results were obtained with ranges of 80.6-98.6% for the recovery, 3.1-10% for the relative standard deviation range, and 9.8-15.6% for the uncertainty. The limits of detection and quantification were 0.015 µg mL(-1) and 0.05 mg kg(-1), respectively. Initial residue concentrations of imidacloprid after the 90 and 180 g a.i. ha(-1) treatments were 0.912 (half-life 11 days) and 1.681 mg kg(-1) (half-life 12.4 days), respectively. For spirotetramat + spirotetramat-enol, the residue concentrations were 1.337 (half-life 5.6 days) and 2.0 mg kg(-1) (half-life 7.6 days) for the 90 and 180 g a.i. ha(-1) treatments, respectively. Spirotetramat degraded faster than spirotetramat-enol. After treatment at 90 g a.i. ha(-1), the initial residues of both insecticides were within European Union maximum residue limits and a 1-day pre-harvest interval (PHI) was adequate for safe consumption of grapes. After treatment at 180 g a.i. ha(-1), the required PHI was 7 day. Therefore, a PHI of 7 day should be used after treatment with imidacloprid and spirotetramat.

Dissipation pattern and risk assessment of flubendiamide on chili at different agro-climatic conditions in India.

Dissipation pattern and risk assessment of flubendiamide and its metabolite (desiodo flubendiamide) on chili were studied at four different agro-climatic locations of India at the standard and double dose at 60 and 120 g a.i. ha(-1) at 10 days interval. Quantification of residues was done on a high-performance liquid chromatograph (HPLC) 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 to be below the determination limit in 15 days at both the dosages in all locations. Half-life of flubendiamide when applied at 60 and 120 g a.i. ha(-1) ranged from 0.85 to 1.80 and from 0.95 to 2.79 days, respectively. 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 use on chili in India by the Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of flubendiamide on chili has been fixed by the Food Safety Standard Authority of India, Ministry of Health and Family Welfare, Government of India, as 0.02 µg g(-1) after its risk assessment.

Persistence and dissipation kinetics of trifloxystrobin and tebuconazole in onion and soil.

The persistence and dissipation kinetics of trifloxystrobin and tebuconazole on onion were studied after application of their combination formulation at a standard and double dose of 75 + 150 and 150 + 300 g a.i. ha(-1). The fungicides were extracted with acetone, cleaned-up using activated charcoal (trifloxystrobin) and neutral alumina (tebuconazole). Analysis was carried out by gas chromatograph (GC) and confirmed by gas chromatograph mass spectrometry (GC-MS). The recovery was above 80% and limit of quantification (LOQ) 0.05 mg kg(-1) for both fungicides. Initial residue deposits of trifloxystrobin were 0.68 and 1.01 mg kg(-1) and tebuconazole 0.673 and 1.95 mg kg(-1) from standard and double dose treatments, respectively. Dissipation of the fungicides followed first-order kinetics and the half life of degradation was 6-6.6 days. Matured onion bulb (and field soil) harvested after 30 days was free from fungicide residues. These findings suggest recommended safe pre-harvest interval (PHI) of 14 and 25 days for spring onion consumption after treatment of Nativo 75 WG at the standard and double doses, respectively. Matured onion bulbs at harvest were free from fungicide residues.

Persistence and dissipation of quinalphos in/on cauliflower and soil under the semi arid climatic conditions of Karnataka, India.

Persistence and dissipation of quinalphos residues in/on cauliflower was studied after giving spray applications at 2 concentrations, i.e. recommended dose of 500 g a.i. ha(-1) and double the recommended dose of 1,000 g a.i. ha(-1). Residue analysis of cauliflower curds was carried out after the third spray over a period of 15 days. Initial residues of quinalphos on cauliflower from the two treatments were 1.19 and 1.842 mg kg(-1). The residues persisted up to 15 days from both the treatments. The residues of quinalphos dissipated from both treatments with the half-life of 4.8 and 5.3 days. Based on the persistence study and maximum residue limit value of 0.05 mg kg(-1) the safe pre-harvest interval was worked out as 17 and 22 days from treatment at the recommended and double the recommended dose, respectively. Analysis of soil samples was carried out on the 15th day of sampling and residues were found to be 0.013 and 0.044 mg kg(-1).

Residue dynamics of fenamidone and mancozeb on gherkin under two agro climatic zones in the state of Karnataka, India.

Residue dynamics of fenamidone and mancozeb on gherkin was evaluated at two different agro climatic zones i.e. at Bangalore (Zone-1) and Dharwad (Zone-2) in the state of Karnataka, India. Two treatments of the combination formulation (fenamidone 10% + mancozeb 50%) were given at the standard dose 150 + 750 g a.i. ha(-1) and double dose 300 + 1,500 g a.i. ha(-1). Initial residue deposits of fenamidone were 0.467 and 0.474 mg kg(-1) at Zone-1 and 2, respectively from standard dose treatment. From double dose treatment they were 0.964 and 0.856 mg kg(-1), respectively. Fenamidone residues persisted for 15 and 10 days and dissipated with the half-life of 4 and 3 days at Zone-1 and 2, respectively. Mancozeb residue deposits on gherkin were 0.383 and 0.428 mg kg(-1) from standard dose and 0.727 and 0.626 mg kg(-1) from double dose treatment at Zone-1 and 2, respectively. Mancozeb residues dissipated with the half-life of 2 and 1 day, respectively. Residues of both fenamidone and mancozeb dissipated faster at Zone-2 compared to Zone-1. The limit of quantification of fenamidone and mancozeb were 0.02 and 0.1 mg kg(-1), respectively in both gherkin and soil. Residues of fenamidone and mancozeb in soil collected on the 20th day from the 2 locations were found to be below quantifiable limit of both fungicides.

An efficient analytical method for analysis of spirotetramat and its metabolite spirotetramat-enol by HPLC.

Spirotetramat is a new compound which belongs to the chemical class of ketoenols. As per the available literature analysis of spirotetramat and its metabolites spirotetramat-enol is carried out by high pressure liquid chromatograph with mass spectrometry (HPLC-MS/MS). In this study we have standardized a method where analysis of both the compounds is carried out by HPLC. The extraction and cleanup of spirotetramat and its metabolites spirotetramat-enol was carried out by QuEChERS method. The cleaned up residues were estimated by HPLC equipped with a photo diode array detector at a wavelength of 250 nm. The mobile phase used was acetonitrile: water at a proportion of 40:60. The limit of quantification (LOQ) of the method was 0.05 mg kg(-1) for both spirotetramat and its metabolite spirotetramat-enol. The recoveries of both the compounds at the LOQ level were in the range of 72.72%-86.76% from mango and 74.82% to 86.92% from cabbage.

Residue dynamics of spirotetramat and imidacloprid in/on mango and soil.

Spirotetramat is a unique insecticide having both phloem and xylem mobility and imidacloprid, a neonicotinoid insecticide, is one of the most widely used in the world. The combination formulation is very effective against sucking pests of mango. Residue dynamics of spirotetramat and imidacloprid in/on mango and soil was studied following application of the combination formulation, spirotetramat 12% + imidacloprid 12% (240 SC) at 90 and 180 g a.i. ha(-1). Spirotetramat residues in/on mango fruits were 0.327 and 0.483 mg kg(-1) after giving 3 applications at 90 and 180 g a.i. ha(-1), respectively. The residues remained on mango fruits for 7 days and dissipated with the half-life of 3.3 and 5.2 days, respectively. Residues of spirotetramat-enol, the major metabolite of spirotetramat in plant, were not detected in mango fruits. Initial residues of imidacloprid on mango fruits from the two treatments were 0.329 and 0.536 mg kg(-1), respectively. Imidacloprid residues remained on mango fruits beyond 15 days and dissipated with the half-life of 5.2 and 8.2 days. The residues of spirotetramat, spirotetramat-enol and imidacloprid were found below quantifiable limit of 0.05 mg kg(-1) in mature mango fruits and field soil at harvest.

Persistence evaluation of fluopyram + tebuconazole residues on mango and pomegranate and their risk assessment.

The persistence of combination formulation of fluopyram 200 + tebuconazole 200-400 SC was evaluated across different agro-climates in India for the management of fungal diseases in two commercially important fruit crops, mango and pomegranate. The residues were extracted using quick easy cheap effective rugged and safe (QuEChERS) method and quantification was done on liquid chromatography-tandem mass spectrometry (LC-MS/MS). The fungicide degradation followed 1st-order kinetics and the half-lives were 2.9-6.4 days for mango, and 3.5-7.4 days for pomegranate for both the fungicides. On the basis of Organisation for Economic Co-operation and Development (OECD) maximum residue limit (MRL) calculation, 1.0 mg kg-1 MRL was obtained for fluopyram while for tebuconazole, it was 0.5 mg kg-1 on mango, at the pre-harvest interval (PHI) of 5 days. For pomegranate, the respective MRLs were 1.0 mg kg-1 and 0.7 mg kg-1 at PHI of 7 days. The dietary risk assessment study indicated that % acceptable daily intake (% ADI) and % acute reference dose (% ARfD) were much lower than 100; thus, the application of fluopyram and tebuconazole on mango and pomegranate is unlikely to present public health concern.

Behavior of beta cyfluthrin and imidacloprid in/on mango (Mangifera indica L.).

Residue persistence of beta cyfluthrin and imidacloprid on mango was carried out after giving spray application of the combination formulation, beta cyfluthrin 9% + imidacloprid 21% (Solomon 300 OD) 3 times at the fruit formation stage. The treatments were, untreated control, standard dose of 75 g a.i. ha(-1) and double dose of 150 g a.i. ha(-1). Initial residues of beta cyfluthrin on mango fruits were 0.04 and 0.12 mg kg(-1) from treatments at the standard and double doses, respectively. The residues dissipated with the half-life of 2.4 and 2.6 days and persisted for 5 days only. Initial residues of imidacloprid on mango fruits were 0.14 and 0.18 mg kg(-1) from treatments at the standard and double doses, respectively. Imidacloprid residues degraded with the half-life of 3.06 and 4.16 days, respectively and persisted for 10 days. Mature mango fruits at harvest were free from residues of both insecticides. A safe pre-harvest interval of 8 days is recommended for consumption of mango fruits after treatment of the combination formulation.

Residue dynamics of tebuconazole and quinalphos in immature onion bulb with leaves, mature onion bulb and soil.

Residue persistence of tebuconazole and quinalphos in immature onion bulb with leaves (spring onion), mature onion bulb and soil was studied following their spray applications 3 times. The applications were untreated control; tebuconazole @ 187.5 and 375 g a.i. ha(-1); quinalphos @ 300 and 600 g a.i. ha(-1). Initial residue deposits of tebuconazole in immature onion bulb with leaves from the two treatments were 0.628 and 1.228 mg kg(-1). The residues of tebuconazole dissipated with the half-life of 5 and 7.7 days. The safe pre-harvest intervals (PHI) for consumption of immature onion bulb with leaves were 16 and 35 days, respectively. Initial residue deposits of quinalphos in immature onion bulb with leaves from the two treatments were 0.864 and 2.283 mg kg(-1). Loss of quinalphos residues from immature onion bulb with leaves was very fast. The residues dissipated with the half-life of 1.7 and 2.6 days and the required PHI was 5 and 11 days, respectively. At harvest mature onion bulbs were free from residues of both tebuconazole and quinalphos.

Residues of acephate and its metabolite methamidophos in/on mango fruit (Mangifera indica L.).

Mango, the major fruit crop of India is affected by stone weevil, which can cause serious damage to the fruits. Acephate gives good control of mango stone weevil. Residues of acephate and its major metabolite, methamidophos were evaluated on mango fruits following repeated spray applications at the recommended dose (0.75 kg a.i. ha⁻¹) and double the recommended dose (1.5 kg a.i. ha⁻¹). Acephate residues mostly remained on the fruit peel which persisted up to 30 days. Movement of residues to the fruit pulp was detected after 1 day of application, increased to maximum of 0.14 and 0.26 mg kg⁻¹ after 3 days and reached to below detectable level (BDL) after 20 days. Methamidophos, a metabolite of acephate, was detected from 3rd day onwards in both peel and pulp and persisted up to 15 days. The residues (acephate + methamidophos) dissipated with the half-life of 5 days in peel and pulp. A safe pre-harvest interval of 30 days is recommended for consumption of mango fruits following treatment of acephate at the recommended dose of 0.75 kg a.i. ha⁻¹.

Persistence and dissipation of fluopicolide in/on grape berries and soil under semi arid tropical climatic conditions of India.

Fluopicolide, a relatively new fungicide is used for control of downy mildew of grape. Persistence study of fluopicolide was carried out on grape berries following treatment of the combination product, fluopicolide 4.44% + fosetyl aluminium 66.7% (Profiler 71.14 WG) at the recommended and double the recommended dose of 2.5 and 5.0 kg ha⁻¹. Four treatment sprays were given at 15 day intervals, starting from 1 month after pruning of the vines. Residues of fluopicolide in grape berries were estimated on 0 (1 h), 1, 3, 5, 7, 10, 15, 20, 25, 30 day and at harvest (64 days after the last spray application). The initial residue deposits of fluopicolide on grape berries were 0.58 and 1.32 mg kg⁻¹ from treatment at the recommended and double dose, respectively. Dissipation of fluopicolide residues was a slow process. After 30 days of treatment, 0.068 and 0.204 mg kg⁻¹ of residues still remained in the berries from treatment at the recommended and double dose, respectively. Fluopicolide residues in grape berries dissipated with the half-life of 10.2 and 12.3 days. Residues in grape berries and soil at harvest were below the quantifiable limit of 0.01 mg kg⁻¹ from both the treatments.

Behavior of acetamiprid, azoxystrobin, pyraclostrobin, and lambda-cyhalothrin in/on pomegranate tissues.

Pomegranate crop is affected by several insect pests and requires usage of a large number of pesticides, but the information on their behavior in pomegranate tissues is limited. A study was conducted to assess the behavior of acetamiprid, azoxystrobin, pyraclostrobin, and lambda-cyhalothrin in pomegranate fruits and leaves. The QuEChERS analytical method and LC-MS/MS and GC-MS were used for quantification of the analytes. The LOD (limit of detection) of acetamiprid, azoxystrobin, and pyraclostrobin was 0.0015 mg kg-1 and lambda-cyhalothrin was 0.003 mg kg-1. The respective LOQ (limit of quantification) was 0.005 and 0.01 mg kg-1. The dissipation of the analytes best fitted into first-order rate kinetics and the half-lives of the chemicals in pomegranate fruits were 9.2-13 days and in the leaves were 13.5-17 days. In the pomegranate aril, the residue levels of acetamiprid, lambda-cyhalothrin, and pyraclostrobin were always < LOQ of these chemicals. Azoxystrobin was detected in pomegranate aril, and its residue was highest at 0.04 mg kg-1 on the 10th day and reached < LOQ by the 25th day. The pre-harvest interval (PHI) required for acetamiprid, azoxystrobin, pyraclostrobin, and lambda-cyhalothrin at standard-dose treatment was 50, 58, 44, and 40 days, respectively. From double-dose treatment, the PHIs were 70, 75, 58, and 54 days, respectively. The pesticides used in this study were more persistent in the pomegranate leaves compared to the fruits. The outcome of this study can be incorporated into production of pomegranate fruits safe for consumption and to meet the domestic and export quality control requirements.