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Pesticide residue analysis of date palm fruits by gas chromatography mass spectrophotometry
Abstract
Pesticides are being used indiscriminately to control insect pests of date palm (Phoenix dactylifera) such as red palm weevil, dubas bug, and mealy bug. The commercial formulation of several pesticides usually applied on date palm as root treatment, or injection into trunk, or as spray on foliage during flowering and fruiting stages to control insect pests. Green fruits of date palm were used for the extraction of pesticides using different solvent extraction procedures. Pesticides extracted from fruits were analyzed on Hewlett Packard gas chromatograph-mass spectrophotometer. Pesticides were identified by using retention time of their reference standard and reconfirmed by HPPEST computer mass spectral library coupled with gas chromatograph-mass spectrophotometer. The residues of dimethoate (0.44 mg/kg fruits) were found 15 days after injection reaching to maximum 1.98 mg/kg after 45 days followed by sharp decline. The trend of accumulation of dimethoate in Aflix insecticide was found similar to that applied alone.
... They found chlorpyrifos and dimethoate concentrations higher than MRLs in three kinds of dates. A survey of pesticide residues in dates in Oman found that the pesticide concentration varies depending on the period of pesticide application and harvest (Khan et al. 2001). Dates are a popular fruit in Arabian countries. ...
A quantitative method based on quick, easy, cheap, effective, rugged, and safe technique (QuEChERS) sample extraction and ultra-performance liquid chromatography/tandem mass spectrometry (UHPLC-MS/MS) was evolved for the determination of 47 pesticide residues in fresh Mazafati date fruits from Bam City of Kerman Province, Iran. The recoveries for selected pesticides ranged from 88 to 110% with a relative standard deviation (RSD) of less than 20% at concentrations of 0.05 and 0.1 mg kg⁻¹. The proposed method had a linear range from the limit of quantification (LOQ) to 1.00 mg kg⁻¹, and the LOQ of the 47 pesticides was ≤ 0.005 mg kg⁻¹. The coefficients of determination (R²) were more than 0.99. This technique was used on 12 fresh date fruits samples, three water samples, and three soil samples with three replications per sample. Forty-seven pesticide were detected collectively, but only diazinon was detected in the date fruit samples. The mean value of diazinon residues was 0.037 mg kg⁻¹, and the concentration of diazinon in most samples was below the national maximum residue limit (MRL) for date fruit (0.05 mg kg⁻¹). Among the pesticides measured, diazinon residues were also detected in the water samples, but not in the soil samples. The dietary intake assessment showed no health risk to humans from the consumption of fresh date fruit concerning the pesticides investigated.
... Previous studies have reported that detected levels of pesticide residues in dates depend entirely on the pesticide application time before harvesting. In an investigation undertaken to analyze the pesticide residues in date fruits in Oman, pesticide accumulation was evident in the first sample (collected 15 days after pesticide application), but the levels were changed in samples collected afterwards and eventually disappeared in 75-day samples and later (Khan et al. 2001). In another study performed on chemical control of pests infesting dates in Iraq, the initial detectable residue levels were decreased about 10 days after pollination, 0-110 7.3 ± 0.9 100 10 Imidacloprid 30 0-98 6.5 ± 0.7 6.6 50 Fig. 4 Application of pesticides to dates. ...
The validation of an analytical procedure based on the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach is presented for multiresidue analysis of pesticides in dates by liquid chromatography-tandem mass spectrometry (UHPLC-MS²). The proposed methodology was applied for simultaneous quantification of 16 pesticides in 50 different date fruits. Method validation was performed regarding accuracy, precision, LDR, LOD, and LOQ, as well as matrix effects. Results of validation were satisfactory, with recoveries higher than 80% for 75% of the samples for 100- and 500- μg L⁻¹ spike levels. Evaluation of the matrix effect revealed that for 81% of the samples, a slight matrix effect was observed. Residues in 92% of the real samples were found below national MRLs. Afterward, hazard quotient (HQ) and total hazard quotient (THQ) of human health risk assessment of pesticides was estimated using a probabilistic approach based on the Monte Carlo (MC) algorithm. Total hazard quotient (THQ) in adults based on the consumption of dates in total samples was estimated to be 7.8% and 36.7% for adults and children, respectively. Since the studied pesticides are registered in the country and are the most widely used pesticides on dates, the occurrence of other pesticide residues seems to be unlikely. Consequently, the applied health risk assessment on Iranian date fruit samples showed that the HQ for adults and children populations indicates no risk to human health.
Graphical abstract
... Insecticides have been banned in many countries including Oman because of their perceived negative environmental effects, such as the pollution of water resources; deterioration of human health; and the resulting reductions in populations of nontarget species, particularly the natural enemies of DB and because of the relatively high application cost (Ansari, Moraiet, & Ahmad, 2014). Studies have shown that some insecticide residues can persist on date palm fruit for up to 2 months after application (Khan, Azam, & Razvi, 2001), which poses a high risk to both humans and animals. Moreover, aerial spraying is difficult to conduct on farms located within mountains, owing to high elevations and valley features (Al-Kindi, Kwan, Andrew, & Welch, 2017a). ...
The Dubas bug (Ommatissus lybicus de Bergevin) is a pest species whose entire life cycle occurs on date palms, Phoenix dactylifera L, causing serious damage and reducing date palm growth and yield. Pseudoligosita babylonica Viggiani, Aprostocetus nr. Beatus, and Bocchus hyalinus Olmi are very important parasitic natural enemies of Ommatissus lybicus in northern Oman. In this study, random farms were selected to (a) model the link between occurrences of the Pseudoligosita babylonica, Aprostocetus nr beatus, and Bocchus hyalinus (dependent variables) with environmental, climatological, and Dubas bug infestation levels (the independent variables), and (b) produce distribution and predictive maps of these natural enemies in northern Oman. The multiple R² values showed the model explained 63%, 89%, and 94% of the presence of P. babylonica, A. nr beatus, and Bocchus hyalinus, respectively. However, the distribution of each species appears to be influenced by distinct and geographically associated climatological and environmental factors, as well as habitat characteristics. This study reveals that spatial analysis and modeling can be highly useful for studying the distribution, the presence or absence of Dubas bugs, and their natural enemies. It is anticipated to help contribute to the reduction in the extent and costs of aerial and ground insecticidal spraying needed in date palm plantations.
... (Aranae: Thomsidae)), and on human health [27]. Research has shown that some pesticide residues can persist on the date fruits for up to sixty days after application [28][29][30]. Furthermore, chemical control measures have met with limited success in Oman, while Dubas bug continues to pose a major challenge to the agricultural industry. ...
Date palm cultivation is economically important in the Sultanate of Oman, with significant financial investment coming from both the government and from private individuals. However, a global infestation of Dubas bug (Ommatissus lybicus Bergevin) has impacted the Middle East region, and infestations of date palms have been widespread. In this study, spatial analysis and geostatistical techniques were used to model the spatial distribution of Dubas bug infestations to (a) identify correlations between Dubas bug densities and different environmental variables, and (b) predict the locations of future Dubas bug infestations in Oman. Firstly, we considered individual environmental variables and their correlations with infestation locations. Then, we applied more complex predictive models and regression analysis techniques to investigate the combinations of environmental factors most conducive to the survival and spread of the Dubas bug. Environmental variables including elevation, geology, and distance to drainage pathways were found to significantly affect Dubas bug infestations. In contrast, aspect and hillshade did not significantly impact on Dubas bug infestations. Understanding their distribution and therefore applying targeted controls on their spread is important for effective mapping, control and management (e.g., resource allocation) of Dubas bug infestations.
... However, Al-Samarrie and Abo-Akela (2011) reported that the residues of CPM were detected after 100 days of injecting the insecticide into the tree's trunk. Long-term persistence of other insecticides was also reported in dates; e.g., dimethoate was detected after 60 days of last injection application into the trunk and disappeared after 75 days (Khan et al. 2001). Residue amounts and the disappearance pattern of FIP are shown in Table 3 and Fig. 1a. ...
Control strategies of red palm weevil (RPW) mainly depend on the use of insecticides. However, the residue of insecticides in dates might cause poisoning risk to the consumers. Therefore, the present study aimed to measure the disappearance rates of the extensively applied insecticides on date palm trees. Residues of chlorpyrifos-methyl (CPM), fipronil (FIP), and imidacloprid (IMD) insecticides in and/or on dates were extracted and cleaned-up using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The residues of CPM, FIP, and IMD were determined by GC-FPD, GC-ECD, and HPLC, respectively. Recoveries of CPM, FIP, and IMD ranged from 86.3 to 98.2%. CPM on dates degraded faster than FIP and IMD. However, after 21 days of the last spray application, 74, 50, and 67% of CPM, FIP, and IMD disappeared, respectively. Residues of CPM and IMD insecticides posed no risk quotient, but FIP caused a risk to humans, depending on the consumption pattern of dates. Insecticides with a fast degradation pattern should be incorporated into the management strategy of RPW to reduce the amount on residues in dates. © 2017 Bundesamt für Verbraucherschutz und Lebensmittelsicherheit (BVL)
... However, these methods are expensive and can have negative environmental impacts on both non-target species, particularly the natural enemies of the DB (e.g., Aprostocetus sp., Oligosita sp., and Runcinia sp.), and on human health [16,17]. Research has shown that some pesticide residues can persist on date fruits for up to 60 days after application [18][19][20]. Moreover, chemical control measures have met with limited success in Oman, where DBs continue to pose a major challenge to the agricultural industry. ...
Date palm cultivation is economically important in the Sultanate of Oman, with significant financial investments coming from both the government and private individuals. However, a widespread Dubas bug (DB) (Ommatissus lybicus Bergevin) infestation has impacted regions including the Middle East, North Africa, Southeast Russia, and Spain, resulting in widespread damages to date palms. In this study, techniques in spatial statistics including ordinary least squares (OLS), geographically weighted regression (GRW), and exploratory regression (ER) were applied to (a) model the correlation between DB infestations and human-related practices that include irrigation methods, row spacing, palm tree density, and management of undercover and intercropped vegetation, and (b) predict the locations of future DB infestations in northern Oman. Firstly, we extracted row spacing and palm tree density information from remote sensed satellite images. Secondly, we collected data on irrigation practices and management by using a simple questionnaire, augmented with spatial data. Thirdly, we conducted our statistical analyses using all possible combinations of values over a given set of candidate variables using the chosen predictive modelling and regression techniques. Lastly, we identified the combination of human-related practices that are most conducive to the survival and spread of DB. Our results show that there was a strong correlation between DB infestations and several human-related practices parameters (R² = 0.70). Variables including palm tree density, spacing between trees (less than 5 x 5 m), insecticide application, date palm and farm service (pruning, dethroning, remove weeds, and thinning), irrigation systems, offshoots removal, fertilisation and labour (non-educated) issues, were all found to significantly influence the degree of DB infestations. This study is expected to help reduce the extent and cost of aerial and ground sprayings, while facilitating the allocation of date palm plantations. An integrated pest management (IPM) system monitoring DB infestations, driven by GIS and remote sensed data collections and spatial statistical models, will allow for an effective DB management program in Oman. This will in turn ensure the competitiveness of Oman in the global date fruits market and help preserve national yields.
... In plantations of palms for fruit production, it is necessary to insure, by carefully fixing the treatment calendar and/or by choosing the right insecticide, that insecticide residue will not be present in the fruit at harvest time. The few available results have shown the absence of residues or their rapid degradation in fruits of various palms after treatment by injection or by absorption through the irrigation water [135]. However, these results have been obtained with insecticides that are no longer used or they are not very conclusive. ...
Introduction. Plants develop mechanisms that allow them to compartmentalize injuries that they suffer during their life. In trees, pruning and injection treatments must be used in accordance with precise rules to reduce risks resulting from the injuries created. Sealing in palms. Palms, contrary to widespread belief, are quite capable of "healing" injuries (sealing); because of an anatomy quite different from trees, the sealing process in palms is much simpler. Compartmentalization of injection wounds. The controversy on the use of injection in trees is due essentially to initial mistakes that have then been rectified. Injection in palms against the red palm weevil. For palms, for decades, this technique has been employed without problems and with great efficiency against various pests, including Rhynchophorus ferrugineus, the red palm weevil (RPW). Its use has been reserved for exceptional situations either to face abnormal pest proliferation, uncontrollable by other techniques, or to implement eradication programs. Integrated eradication program. In such a program, the main aim of injection treatments is preventive. With long-persistence insecticides, the number of treatments could be greatly reduced. The resulting savings in time and money would enable the organization of the treatments of all the palms located in an infested area, and consequently the rapid eradication of the pest. New perspectives. We established that insecticides applied by injection were capable of protecting palms with only two or even one treatment per year. These results suggest a radical improvement in programs to eradicate RPW, while considerably reducing the risks to health and the environment compared with spray treatments.
... In plantations of palms for fruit production, it is necessary to insure, by carefully fixing the treatment calendar and/or by choosing the right insecticide, that insecticide residue will not be present in the fruit at harvest time. The few available results have shown the absence of residues or their rapid degradation in fruits of various palms after treatment by injection or by absorption through the irrigation water [135]. However, these results have been obtained with insecticides that are no longer used or they are not very conclusive. ...
Introduction. Plants develop mechanisms that allow them to compartmentalize injuries that they suffer during their life. In trees, pruning and injection treatments must be used in accordance with precise rules to reduce risks resulting from the injuries created. Sealing in palms. Palms, contrary to widespread belief, are quite capable of “healing” injuries (sealing); because of an anatomy quite different from trees, the sealing process in palms is much simpler. Compartmentalization of injection wounds. The controversy on the use of injection in trees is due essentially to initial mistakes that have then been rectified. Injection in palms against the red palm weevil. For palms, for decades, this technique has been employed without problems and with great efficiency against various pests, including Rhynchophorus ferrugineus, the red palm weevil (RPW). Its use has been reserved for exceptional situations either to face abnormal pest proliferation, uncontrollable by other techniques, or to implement eradication programs. Integrated eradication program. In such a program, the main aim of injection treatments is preventive. With long-persistence insecticides, the number of treatments could be greatly reduced. The resulting savings in time and money would enable the organization of the treatments of all the palms located in an infested area, and consequently the rapid eradication of the pest. New perspectives. We established that insecticides applied by injection were capable of protecting palms with only two or even one treatment per year. These results suggest a radical improvement in programs to eradicate RPW, while considerably reducing the risks to health and the environment compared with spray treatments.
... (Vig et al., 1995;Rizos, 1994;Khan et al., 2002;Cabras et al., 1993) (Fillion et al., 1995;Zwick et al., 1977;Lee and Westcott, 1981;Prieto et al., 1999;Ferreira et al., 1987;Hegazy et al., 1999;Hiskia et al., 1998;Parkash and Verma, 1983;Iwata et al., 1979). (Meloan, 1996) : (Timme and Frehse, 1980) . ...
This study was carried out at Abou Jarash farm, Faculty of Agriculture, Damascus University, to study the stability of dimethoate residues and its oxygen–analogue metabolites (omethoate) in olives at the recommended application rate of 100 ml/100 liter water of dimethoate 40% EC on olive trees. Samples were collected after application which extended to 25 days, then transferred to the laboratory after putting them in polyethylene bags, and the whole preparation procedures were applied to conduct the analysis by gas chromatography. Dimethoate residues in olive fruits was 9.264 mg/kg after one–hour post treatment, and then decreased to 0.723 mg/kg after 25 days of application. The results showed that the pesticide dissipation has gone through two main stages. The first is the relative sharp dissipation stage during the first 10 days after application. In the second stage, the dissipation was relatively slow. The line regression of dimethoate degradation in olives took a first- order reaction, also the remaining deposit of 0.723 mg/kg after 25 days was above the recommended MRL=0.5 mg/kg on olives. The dimethoate half-life on olives was 8.4 days and the calculated pre-harvest interval (PHI) was 53.7 days, whereas the PHI as stated by the manufacturing company was 21 days. This study also showed that the persistence of omethoate in olives was observed at the beginning of application until the end of the sampling period 25 days post treatment. The residue quantities ranged from 0.84 to 0.36 mg/kg in olives
(8) (PDF) Persistance of Dimethoate Residues in Olive Fruit under field conditions. Available from: https://www.researchgate.net/publication/260006666_Persistance_of_Dimethoate_Residues_in_Olive_Fruit_under_field_conditions [accessed Oct 13 2021].
The aim of this study was to develop a convenient, fast, effective and safe analytical method (QuEChERS) to determine 198 pesticide residues in multi-source date palm fruits using gas chromatography-tandem mass spectrometry (GC-MS/MS). The calibration curves for most pesticides were linear in the range of 15-150 µg/kg, with r2 values higher than 0.9934 and the relative standard deviation for all pesticides was ≤20%. The mean recovery rate of pesticides was 70-120% and limits of detection (LODs) and limits of quantification (LOQs) were in the range of 5-14 µg/kg and 14-40 µg/kg, respectively. The validated procedure was used to monitor pesticide residues in 30 fresh date samples. It could be concluded that the modified QuEChERS extraction method was efficient in analysing pesticide residues in dates palm and none of the samples contained residues above the MRLs.
In order to understand the distribution and prevalence of Ommatissus lybicus (Homoptera: Tropiduchidae) as well as analyse their current biographical patterns and predict their future spread, comprehensive and highly sophisticated information on the environmental, climatic, and agricultural practices are essential. The analytical techniques available in modern spatial analysis packages, such as Remote Sensing and Geographical Information Systems, can help detect and model spatial links and correlations between the presence, absence and density of O. lybicus in response to climatic, environmental and human factors. The main objective of this paper is to review remote sensing and geographical information analytical techniques that can be applied in mapping and modelling the habitat and population density of O. lybicus in Oman. An exhaustive search of related literature revealed that there are few studies linking location-based infestation levels of pests like the O. lybicus with climatic, environmental and human practice related variables in the Middle East. Our review also highlights the accumulated knowledge and addresses the gaps in this area of research. Furthermore, it makes recommendations for future studies, and gives suggestions on monitoring and surveillance sites that are necessary in designing both local and regional level integrated pest management (IPM) policing of palm tree and other affected cultivated crops.
Larvae of the lesser date moth (Batrachedra amydraula Meyr.) cause damage to dates in Iraq. A formulation based on a mixture of equal parts of wheat flour and pollen grains and containing either chlorpyrifos, fenitrothion or pirimiphos-methyl (all at 5 mg kg−l) was dusted (5 g formulation bunch−1) onto female clusters of dates at the time of pollination. Numbers of larvae, yield of dates and insecticide residues were monitored over a three-month period. Results showed that, by this technique, all three insecticides were effective in controlling the pest but that fenitrothion and chlorpyrifos were better than pirimiphos-methyl.
A procedure based on current multi-residue methodology is described for the determination of synthetic pyrethroid residues in vegetable and animal tissues. Permethrin, cypermethrin, and fenvalerate are extracted from celery, egg yolk, beef muscle, and milk with acetonitrile, partitioned into hexane, and cleaned up on Florisil for quantitation by electron capture gas chromatography. Recoveries of the 3 pyrethroids averaged 94-103% from celery and 82-97% from animal products. Minimum detectable levels of less than 5 ng/g are readily attainable. The method also allows for the simultaneous extraction and cleanup of the organochlorine hydrocarbon insecticides which have been routinely analyzed in the past.
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