Pesticide Residues In Foodstuffs Research Articles

Improved analysis of 230 pesticide residues in three fermented soy products by using automated one-step accelerated solvent extraction coupled with GC–MS/MS

Consumer concerns over healthy diets are increasing as a result of the toxicity and persistence of pesticide residues in foodstuffs. Developing sensitive and high-throughput monitoring techniques for these trace residues is seen as an essential step in ensuring food safety. An automatic and sensitive multi-residue analytical method was developed and validated for the simultaneous determination of 230 compounds, including pesticides and their hazardous metabolites, in fermented soy products. The method included preparing the sample using on-line extraction and clean-up system based on accelerated solvent extraction (ASE), then determining the analytes using GC–MS/MS techniques. The homogenized samples (soy sauce, douchi, and sufu) were automatically extracted at 80 °C and 10.3 MPa and at the same time, in situ cleaned by 300 mg of primary secondary amine (PSA) combined with 20 mg of hydroxylated multi-walled carbon nanotubes in an extraction cell. The method obtained excellent calibration linearity (r > 0.9220) and a satisfactory analysis of the targeted compounds, which were evaluated with matrix-matched calibration standards over the range of 5–500 μg L−1. The limit of detections (LODs) of analytes were in the range of 0.01–1.29 μg kg−1, 0.01–1.39 μg kg−1, and 0.01–1.34 μg kg−1 in soy sauce, douchi, and sufu, respectively. The limit of quantifications (LOQs), which defined as the lowest spiking level, were set at 5.0 μg kg−1. The recoveries were within 70–120 % for over 95 % of the analytes, and the relative standard deviations (RSDs) were below 13.6 %. Moreover, a positive detection rate of 47 % were obtained when the proposed method was used on 15 real fermented soy products. These results suggested that the developed high-throughput method is highly feasible for monitoring of these target analytes in trace level.

Pesticide contamination pattern from Morocco, insights into the surveillance situation and health risk assessment: a review.

The widespread application of pesticides in Morocco's agriculture renders their monitoring in food and environmental samples very necessary. Recent years have witnessed a growing interest in reporting studies related to the monitoring of pesticide residues in food, water, groundwater, and soil as well as their quantitative health risk assessment. Most published studies have been done by university researchers. However, the lack of research reproducibility remains a problem that considerably limits the possibility of exploiting data from the literature. Our study involves an extensive literature review utilizing search engines with keywords like "pesticide residues," "monitoring," "vegetables and fruits," "water and soil," "risk assessment," and "Morocco" from 2009 to 2023. Analysis of pesticide residues in foodstuffs and environmental samples highlights concerns over compliance with EU regulations, the health risks associated with pesticide exposure, and the necessity for comprehensive monitoring and risk assessment strategies. This paper could help influence policies to develop a strategy and action plan for the sound management of pesticides, including measures to reduce their use, raise awareness, and monitor compliance. Also, this paper could be useful for scientists interested in understanding the current situation and challenges regarding pesticide residues in Morocco, as well as countries with which commercial links exist.

Preparation and extraction property study of corn cob-like magnetic mosaic carbon materials derived from MOF-on-MOF composites

BackgroundLarge accumulations of pesticide residues in the environment eventually enter the human body with food. Based on magnetic solid-phase extraction (MSPE) technology, it is possible to achieve efficient extraction of trace pesticide residues in foodstuffs, and the construction of MSPE adsorbents with excellent magnetic properties and many active sites is still one of the main research topics. Based on this, we developed a new strategy for the preparation of "MOF-on-MOF" composites, which were carbonized and used as adsorbents for the extraction of pesticide residues in cereals. ResultsA novel corn cob core-shell composite Fe2O3@C@ZIF-8 was created by embedding ZIF-8 onto the surface of Fe2O3@C derived from MIL-88A(Fe), and used for the extraction of benzoylurea insecticides(BUs) from cereals. The adsorption behaviour between Fe2O3@C@ZIF-8 and BUs was investigated by static and kinetic experiments and the adsorption mechanism was elaborated. For the trace analysis of BUs, a magnetic solid-phase extraction combined with high performance liquid chromatography-ultraviolet detector (HPLC-UV) approach was also developed. Under the optimized experimental conditions, the limits of detection and quantification were 0.015–0.03 μg L−1 and 0.05–0.1 μg L−1, and the relative standard deviations for the intra-day and inter-day ranges were 1.82%–2.13 % and 3.85%–4.59 %, respectively. The spiked recoveries of the four cereals ranged from 82.72% to 104.45 %. After 10 cycles of use of Fe2O3@C@ZIF-8, the recoveries of BUs ranged from 77.90% to 96.74 %. SignificanceThe analytical method based on Fe2O3@C@ZIF-8 as adsorbent has a low limit of detection, a wide linear range and is highly applicable to the analysis of real samples. In addition, the strategy developed in this study for the preparation of thermoplastic polymer-assisted "MOF-on-MOF" composites has promising applications.

Different types of pesticide residues in foodstuffs

Pesticide have contributed greatly to increase of yield in agriculture by controlling pests. The staggering of agriculture that has has been achieved so far has been driven by pesticide. It has negative impacts for the whole ecosystem by entering food residues. Food products were found to have contaminated 51 percent with pesticide residues were higher than the MRL. The present research was carried out to measure the concentration and awareness of pesticide residues in food stuffs and to quantify the possible health hazards linked with pesticide residue. GC-ECD/NPD was used to estimate the pesticide residues. Analysis of four common organophosphate pesticides chloropyriphos, dimethoate, profenofos, quinalphos and phorate are widely applied on fruits and vegetables was carried out. Along with this residue levels of four pyrethroid and carbamate in fruits and vegetables samples were analysed. In order to analyze the residue levels in major foodstuffs in Kerala, samples of fruits and vegetables have been collected from markets located in Thiruvananthapuram and Kasargod.

Analysis of Pesticide Residues in Water, Rice, Fruits and Vegetables

Pesticides have played a major role in increasing agricultural output by pest control and eliminating insect driven illnesses. Kerala’s tragedy on endosulfan exposure made us to study pesticides in water, rice, fruits and vegetables from Thiruvananthapuram location. Rice (the main cereal consumed in Kerala), fruits, and vegetables, as well as water samples from wells and streams in the Thiruvananthapuram districts, were collected for analysis of residue levels in major food items consumed by people in Kerala. The research was carried out to measure the concentration of organochlorine, organophosphorus, and synthetic pyrethroid pesticides using gas chromatography. The water and food samples collected were analysed for pesticide residues and the quantities were estimated using GC-ECD/NPD. A standard mixture containing Pesticides (OCs, OPs, Pyrethroids, and carbamates) was run before the actual samples. The detection was used to estimate the residues of fifteen commonly used pesticides, namely organochlorine pesticides (endosulfan, dieldrin, aldrin, lindane, DDT), organophosphorus pesticides (chlorpyrifos, profenophos, quinalphos, dimethoate, phorate) and synthetic pyrethroid pesticides (cypermethrin, fenvalerate, deltamethrin, carbofuran). The study concluded that food exposure to pesticides would result in unacceptable health hazards and awareness of pesticide residues in foodstuffs, as well as to quantify the possible health. Hence, necessary to maintain the survey of pesticide residues in all food commodities in order to safeguard the consumers.

Analisis Kualitatif Residu Pestisida Pada Bahan Pangan Dengan Menggunakan Metode Kromatografi Lapis Tipis (KLT)

Vegetables and fruits are foodstuffs whose cultivation process requires pesticides. In addition to farmers who apply pesticides, pesticide poisoning can also be experienced by people who consume agricultural products including vegetables through the pesticide residues contained in them, so that it will have a negative impact on human health who consume them continuously. The purpose of the study was to determine the presence of pesticide residues in foodstuffs. This research is a laboratory observation with a simple random sampling technique. In this study, a qualitative analysis of organophosphate and carbamate pesticide residues in food ingredients was carried out using the Thin Layer Chromatography (TLC) method. Based on the results of the study, from 15 (fifteen) samples of vegetables, no organophosphate chlorpyrifos pesticide content was detected, but the carbamate group was detected in samples of spinach, cabbage, and carrots marked with spots and the Rf value was the same as the Furadan standard. Thus, it is hoped that the community will wash the vegetables before they are processed and consumed.

Multi-Residue Screening of Pesticides in Aquaculture Waters through Ultra-High-Performance Liquid Chromatography-Q/Orbitrap Mass Spectrometry

Pesticide residues in foodstuffs can lead to several undesirable effects. A simple and high-throughput targeted screening method analyzing multi-residue pesticide in aquaculture water based on ultra-high-performance liquid chromatography-Q/Orbitrap mass spectrometry (UHPLC-Q/Orbi MS) was developed and validated. In this technique, the peaks of the compound using precursor ions were recorded by the full scan, which was used for rough quantitative analysis with single point matrix matched calibration. The qualitative identification was performed following the stringent confirmation criteria with fragment ions, retention time, and an isotopic pattern. Additionally, solid-phase extraction with an HLB (Hydrophilic/Lipophilic Balanced) column was selected to enrich and separate target pesticides from water. The screening detection limit of 33 compounds are less than 2 ng·L−1, while 26 compounds range from 2 ng·L−1 to 10 ng·L−1, 19 compounds are at the range of 10–200 ng·L−1, and the other two compounds are 200 ng·L−1 and 1000 ng·L−1. Most of the recovery results were found to be between 60~130%. Finally, the method was successfully applied to the analysis of pesticide residues in 30 water samples from aquaculture environment in Shanghai, indicating its applicability in pesticide screening for environmental monitoring.

Evaluation of the reproducibility standard deviation in the pesticide multi-residue methods on olive oil from past proficiency tests

The data reported in the frame of proficiency testing (PT) exercises organized from 2007 to 2016 have been statistically re-evaluated using Algorithm A of the ISO 13528:2015, and the relative standard deviation for reproducibility of multi-residue methods for the determination of pesticides in olive oil was evaluated. Usually, the assigned between-laboratories variability in PTs on pesticide residues is fixed/set to 25 %. This value was compared to the calculated robust relative standard deviation (RRSD). A total of 1527 analytical results were collected in the ten PTs for the determination of pesticides in olive oil. An RRSD of 21 % was obtained, below the maximum value of 25 %. If all participants use the same analytical approach (e.g., multi-residue method and same instrumental technique), a lower value of the reproducibility standard deviation should be expecting. The QuEChERS method, coupled with LC–MS/MS and GC–MS/MS, has become an important methodology for the analysis of pesticide residues. This is due to its simplicity, the use of low quantities of acetonitrile, the possibility to analyze a large number of pesticides with fewer steps and high efficiency. This method may harmonize the future of pesticide residue analyses. Recently, it was successfully applied to the analysis of olive oil by 70 % of the laboratories participating to our last PT exercise. An expanded uncertainty of 50 % was systematically applied in Europe since 2006 for the analyses of pesticides; the use of the QuEChERS methodology may reduce to 40 %. This work could contribute to promote the comparability of measurements of pesticide residues in foodstuffs.

Silica-based magnetic hybrid nanocomposite for the extraction and preconcentration of some organophosphorus pesticides before gas chromatography.

The precise control of pesticide residues in foodstuffs depends significantly on the clean extraction of analytes using specifically designed separation methods. In this study, a one-pot sol-gel process was used for the preparation of a magnetic hybrid silica gel tetraethylortho silicate-cyanopropyltriethoxy silane nanocomposite. The prepared material was characterized using energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, single-point specific surface area, and scanning electron microcopy. The synthesized magnetic hybrid material was used as a solid phase extraction sorbent for the extraction and preconcentration of some organophosphorus pesticides before gas chromatography with a microelectron capture detector. The performance of the proposed magnetic solid-phase extraction technique was validated by linearity (0.05-2ng/mL), correlation coefficients (r2 =0.9993-0.9997), limit of detection (0.02-0.06ng/mL, S/N=3, n=3), and intraday (RSD=1.5-8.7%, n=3) and interday precision (RSD=5.5-9.3%, n=12), while the recovery in real samples and equilibrium adsorption capacity was 72.02-103.84% and 8-20mg/g, respectively. The magnetic solid-phase extraction based on the hybrid nanocomposite revealed a high enrichment factor, an appropriate dynamic range, and great absorptive ability toward the selected organophosphorus pesticides spiked in real water samples.

Roller conveyer system for the reduction of pesticides using non-thermal gas plasma - A potential food safety control measure?

We previously described a novel roller conveyer plasma device, which generates gas plasma via atmospheric pressure dielectric barrier discharge, to disinfect vegetables in situ during the sorting process. Here, we tested this system to verify whether or not such treatment was also effective in pesticide reduction. Competitive enzyme-linked immunosorbent assay showed the pesticide malathion, present at levels typically observed on treated crops, was efficiently degraded to less than one tenth of the original level within 1 min. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) confirmed the decrease in the level of pesticide cocktail PL-14-2 and FA-2, including organophosphorus pesticides and other classes of pesticides, after plasma treatment. A cholinesterase inhibitory activity assay was used as an index to measure the activity of PL-14-2 and FA-2, which showed that the gas plasma treatment reduced the biological activity of the pesticides. In addition to its proven biocidal effects, our findings demonstrate the potential of this non-thermal plasma system as a food safety control measure ensuring reduction of pesticide residues in foodstuffs.

Effective Monitoring of Fluxapyroxad and Its Three Biologically Active Metabolites in Vegetables, Fruits, and Cereals by Optimized QuEChERS Treatment Based on UPLC-MS/MS

Qualitative analysis and quantification of pesticide residues in foodstuff are essential to our health in daily life, especially regarding their metabolites, which may be more toxic and persistent. Thus, a valid analytical measure for detection of fluxapyroxad and its three metabolites (M700F002 (C-2), M700F008 (C-8), M700F048 (C-48)) in vegetables (cucumber, tomato, and pepper), fruits (grape, apple), and cereals (wheat, rice) was developed by UPLC-MS/MS with negative ion mode. The target compounds were extracted by acetonitrile contain 0.2% formic acid (v/v), and the extractions were cleaned up by octadecylsilane sorbents. The limits of quantitation and quantification were less than 0.14 μg kg-1 and 0.47 μg kg-1 in seven matrices. Furthermore, recoveries at levels of 0.01, 0.05, and 0.1 mg kg-1 ranged from 74.9% to 110.5% with relative standard deviations ≤15.5% (n = 5). The method is validated to be effective and robust for the routine supervising of fluxapyroxad and its metabolites.

Dichloro-diphenyl-trichloro-ethane (DDT) and hexachlorohexane (HCH) pesticide residues in foodstuffs from markets in Ile-Ife, Nigeria

Levels of dichlorodiphenyltrichloroethanes (DDTs) and Hexachlorocyclohexanes (HCHs) pesticide were evaluated in samples of cowpea grains and dried yam chips obtained from Ile-Ife markets, southwestern Nigeria. The objectives of the study were to establish the presence of the organochlorine pesticide residues in the foodstuffs and also to ascertain whether the residue levels are above their respective permissible levels. Randomly selected samples from highly patronized markets were subjected to standard extraction protocols. The DDT and HCH levels were determined using Gas Chromatography coupled with Electron Capture Detector (GC-ECD). The mean concentration of ϒ-HCH (Lindane) in cowpea grains was 0.085 mg/kg and 0.042 mg/kg in dried yam chips. The ρ,ρ’-DDD concentrations were 0.086 mg/kg and 0.159 mg/kg in cowpea and dried yam chips, respectively. ϒ-HCH detected in all the cowpea samples and 90% in dried yam chips samples were above the recommended EU maximum residue level (MRL) of 0.01 mg/kg. The results of this study indicated that substances that could pose serious health risks were associated, at outrageous levels, with important foodstuffs in Nigerian markets even to the point of sales and consumption. Keywords : Dichlorodiphenyltrichloroethane, hexachlorocyclohexane, pesticide, residue, cowpea grain, yam chip.

National summary reports on pesticide residue analysis performed in 2013

EFSA Supporting PublicationsVolume 12, Issue 3 755E Technical reportOpen Access National summary reports on pesticide residue analysis performed in 2013 European Food Safety Authority (EFSA), European Food Safety Authority (EFSA)Search for more papers by this author European Food Safety Authority (EFSA), European Food Safety Authority (EFSA)Search for more papers by this author First published: 12 March 2015 https://doi.org/10.2903/sp.efsa.2015.EN-755 Published date: 12 March 2015 Question number: EFSA-Q-2015-00057 AboutPDF ToolsExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL References EFSA (European Food Safety Authority) 2014. Use of the EFSA Standard Sample Description for the reporting of data on the control of pesticide residues in food and feed according to Regulation (EC) No 396/2005 (2013 Data Collection). EFSA Journal 2014; 12(1):3545, 60 pp. doi:10.2903/j.efsa.2014.3545 EFSA (European Food Safety), 2015. The 2013 European Union report on pesticide residues in food. EFSA Journal 2015; 13(3):4038, 170 pp. doi:10.2903/j.efsa.2015.4038 EU (European Commission), 2004. Notification criteria for pesticide residue findings to the Rapid Alert System for Food and Feed. SANCO/3346/2001, revision 7. EU (European Commission), 2009. Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed. SANCO/10684/2009. EU (European Commission), 2011. Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed. SANCO/12495/2011. ISO/IEC (International Organization for Standardization and the International Electro-technical Commission), 2010. General requirements for the competence of testing and calibration laboratories. 17025:2005, 28p. Maudoux J-P, Saegerman C, Rettigner C, Houins G, van Huffel X and Berkvens D, 2006. Food safety surveillance by a risk based control programming: approach applied by the Belgian federal agency for the safety of the food chain. Veterinary Quarterly, 28(4), 140– 154. Petersen A, Hamborg B, Andersen J H, Poulsen M E, Christensen T, Nielsen E, 2013. Pesticides residues, results from the period 2004–2011. ISBN 978-87-92763-78-5. The Netherlands' General Inspectorate for Health Protection, Ministry of Public Health, Welfare and Sports, 1996. Analytical Methods for Pesticide Residues in Foodstuffs. 6th Ed. Volume12, Issue3March 2015755E ReferencesRelatedInformation

Biological Management of Damping-Off, Buckeye Rot and Fusarial Wilt of Tomato (cv. Solan Lalima) under Mid-Hill Conditions of Himachal Pradesh

Disease management is often complicated by the presence of multiple types of pathogens; in an organic system, it is appropriate to develop disease control strategies. The available literature so far reflects that the management of important disease of tomato is through the integrated approaches and very few organic approaches have been tried with various degree of success. Boiopriming of seeds with biocontrol agents (Trichoderma viridae, Trichoderma harzianum and Pseudomonas fluorescens) in combination with different biofertilizers (Azotobacter, Azospirillum and PSB) and organic manures (FYM and vermi-compost) were tested against disease incidence and health management of tomato seedling under nursery as well as field conditions. The studies were conducted during two successive years (2012-2013) at farmer’s field with the objective to combat with the increasing disease incidence of three major disease damping-off, fusarium wilt and buckeye rot from nursery stage to the final harvesting. The study focused on the use of biocontrol agents as the suitable alternative to chemical pesticides with sustainable disease management without pesticide residues in foodstuff. The bio priming of seeds with fungal antagonist Trichoderma viridae and harzianum and bacterial antagonist Pseudomonas fluorescens significantly improved the germination behavior of tomato seeds as compared to untreated control. Highest mean germination (93.1%) and seedling vigour (953.33) was recorded in Treatment 3 (FYM @ 200 q/ ha + Azospirillum + PSB + Trichoderma herzianum (4 kg/ha each) and lowest in control (60.3%) and (304.83), thus indicating a significant per cent increase in seedling emergence (54.4%) and seedling vigour (95.23%). A considerable reduction in disease incidence (pre and post) of damping off was observed in treatment T? and T? (VC @ 50 q/ha + Azospirillum + PSB + Trichoderma herzianum @ (4 kg/ha) with 45.6% and 35.4% respectively). Treatment T? proved highest in terms of yield (665 Kg/Ha), Hence these diseases can be managed by successful application of Biocontrol agents.

National summary reports on pesticide residue analysis performed in 2012

EFSA Supporting PublicationsVolume 11, Issue 12 700E Technical reportOpen Access National summary reports on pesticide residue analysis performed in 2012 European Food Safety Authority (EFSA), European Food Safety Authority (EFSA)Search for more papers by this author European Food Safety Authority (EFSA), European Food Safety Authority (EFSA)Search for more papers by this author First published: 11 December 2014 https://doi.org/10.2903/sp.efsa.2014.EN-700 Published date: 11 December 2014 Question number: EFSA-Q-2014-00835 AboutPDF ToolsExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat References EFSA (European Food Safety Authority), 2013. Use of the EFSA Standard Sample Description for the reporting of data on the control of pesticide residues in food and feed according to Regulation (EC) No 396/2005 (Revision 2). EFSA Journal 2013; 11(1):3076, 54 pp. doi:10.2903/j.efsa.2013.3076. EFSA (European Food Safety Authority), 2014. The 2012 European Union Report on Pesticide Residues in Food. EFSA Journal 2014 – to be completed. EU (European Commission), 2004. Notification criteria for pesticide residue findings to the Rapid Alert System for Food and Feed. SANCO/3346/2001, revision 7. EU (European Commission), 2009. Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed. SANCO/10684/2009. EU (European Commission), 2011. Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed. SANCO/12495/2011. ISO/IEC (International Organization for Standardization and the International Electro-technical Commission), 2010. General requirements for the competence of testing and calibration laboratories. 17025:2005, 28p. Maudoux J-P, Saegerman C, Rettigner C, Houins G, van Huffel X and Berkvens D, 2006. Food safety surveillance by a risk based control programming: approach applied by the Belgian federal agency for the safety of the food chain. Veterinary Quarterly, 28(4), 140– 154. The Netherlands' General Inspectorate for Health Protection, Ministry of Public Health, Welfare and Sports, 1996. Analytical Methods for Pesticide Residues in Foodstuffs. 6th Ed. Petersen A, Hamborg B, Andersen J H, Poulsen M E, Christensen T, Nielsen E, 2013. Pesticides residues, results from the period 2004–2011. ISBN 978-87-92763-78–5. Volume11, Issue12December 2014700E ReferencesRelatedInformation

Pesticide residues in fruits and vegetables from Pakistan: a review of the occurrence and associated human health risks.

The main objective of the review is to document, assess and analyze the results of the previously reported data on levels of different pesticides in selected fruits and vegetables from Pakistan. The findings of the previous studies clearly indicated that more than 50 % of the samples were contaminated with organophosphate, pyrethroids and organochlorine pesticides. Many studies reported that among fresh fruits and vegetables tomato, apple, melon, mango, grapes, and plum crossed the FAO/WHO permissible limits for these contaminants residual levels. The comparison of other regions showed that observed levels were found above maximum residue limits (MRLs) in 50 % of the samples but were in agreement with the studies from neighboring countries like China and Bangladesh. Higher hazard risk index (HRI) values were calculated for dieldrin, methamidophos, o,p'-DDT, diazinon and p,p'-DDT in apple, mango, banana, melon, potato and onion. The review also highlights that data on pesticide residues in foodstuff is scarce which should be overcome by further extending studies from different areas of Pakistan. In order to ascertain the provision of food suitable for human consumption, it is imperative to monitor pesticides in food commodities by the country's authorities and enforce guidelines based on permissible limits.

Method development for directly screening pesticide residues in foodstuffs using ambient microfabricated glow discharge plasma (MFGDP) desorption/ionization mass spectrometry

An innovative method for directly screening pesticide residues in foodstuffs was developed using ambient microfabricated glow discharge plasma (MFGDP) desorption/ionization mass spectrometry. The capability of qualitative and quantitative analysis with MFGDP–MS at atmospheric pressure on agrochemicals has been demonstrated. Nine multi-class compounds (ametryn, amitraz, buprofezin, dimethoate, diphenylamine, imazalil, isoproturon, malathion, parathion-ethyl) were examined in spiked solutions, in extracts of fruits and vegetables, and in unprocessed samples. In the standard solutions of the nine pesticides, the application of MFGDP-MS for the detection of organophosphorus, organochlorine and organonitrogen compounds was demonstrated. Limits of detection (LODs) at levels down to 0.13ngg−1mm−2 of the spiked extracts of tomato, green pepper, and orange (collected by “QuEChERS”) were obtained, with RSDs of 3.48–13.46%. In the direct analysis of unspiked peels and extracts of apple, celery and grapes, the residues of diphenylamine, dimethoate and malathion were successfully analyzed by tandem mass spectrometry (MS/MS). The distribution of diphenylamine in apples was obtained by scanning the various unprocessed parts of the apple piece-by-piece in depth directly. Thus, an MFGDP–MS, having a small size and operating at a low temperature, made it possible to directly and accurately screen for pesticide residues in fruits and vegetables in situ.

Development and validation of a grouping method for pesticides analysed in foodstuffs

The cost effective monitoring of hundreds of pesticide residues in foodstuffs of vegetable origin involves the definition of groups of analytes associated with homogeneous performance parameters of the used analytical method. The performance of the analytical method only needs to be tested on a daily base for some of these group's compounds. This work proposes a strategy for defining groups of compounds with homogeneous physical-chemical properties based on the evaluation of the similarity of the multivariate pattern of five of these properties namely: molar mass, melting point, vapour pressure at 20 °C, n-octanol-water partition coefficient and solubility in water at 20 or 25 °C. Three independent and competing multivariate analysis tools, namely Principal Component Analysis, Hierarchical Clustering and K-Mean Clustering were used. This strategy was successfully used to group 100 pesticides into nine clusters, with 1-40 pesticides, represented by a compound with within group average properties. The developed grouping method was validated using physical-chemical data from other references or compounds and produced groups consistent with the performance of the studied determination of pesticide residues in dried red bean. The mean analyte recoveries of groups with larger dimension are statistically different for a confidence level of 95%. The within group coefficients of variance of mean analyte recoveries of larger groups ranged from 6.7% to 8.5%. This grouping method can reduce the number of recovery tests performed for the validation of the analytical method or test quality control.

Compatibility of Different Insecticides with Trichoderma harzianum Under in vitro Condition

Trichoderma spp. are also known as effective bio-control agents against soil-borne pathogens of several important crops. Integration of chemicals and bio-control agents has been the subject of research during recent years. The potential value of bio-pesticides for the control of important plant pathogens requires investigation due to the general requirement for very low pesticide residues in foodstuffs and concerns over the increasing development of resistance to the different classes of chemicals. The aim of the present study was to check the compatibility of different insecticides viz., Decis (deltamethrin 2.8% EC), Ekalux EC 25 (quinalphos 25% EC), Fenval 20% EC (fenvalerate 20% EC), Hilcron 36 SL (monocrotophos 36 SL), Hildan 35 EC (endosulfan 35 EC), Hilmida (imidacloprid 17.8 SL), Marshal 25 E (carbosulfan 25% EC), Rogor 30% EC (dimethoate 30% EC), Rocket 44 EC (profenofos 40%+cypermethrin 4%) with V15 strain of Trichoderma harzianum Rifai. Mycelial growth of V15 strain of Trichoderma harzianum was calculated in the presence of above mentioned insecticides by using Potato Dextrose Broth (PDB) medium and SP3 medium separately. Hilmida (imidacloprid 17.8 SL) was found to be most compatible with V15 strain of Trichoderma harzianum in both the liquid media as it shows nil percentage reduction of mycelium. It was concluded that conclude that Decis (deltamethrin 2.8% EC), Hilcron 36 SL (monocrotophos 36 SL), Hilmida (imidacloprid 17.8 SL) and Rogor 30% EC (dimethoate 30% EC) are compatible insecticides with biocontrol agent (Trichoderma harzianum) while some insecticides viz., Ekalux EC 25 (Quinalphos 25% EC), marshal 25 E (carbosulfan 25% EC) and rocket 44 EC (profenofos 40%+cypermethrin 4%) inhibits the growth of Trichoderma spp.

Determination at low ppm levels of dithiocarbamate residues in foodstuff by vapour phase-liquid phase microextraction-infrared spectroscopy

A methodology based on the vapour phase (VP) generation of carbon disulphide from non-volatile dithiocarbamate compounds has been developed for determination of pesticide residues in foodstuff at low ppm levels. The method involves a selective reaction combined with liquid phase microextraction (LPME) and transmission infrared measurements. The use of a home made transmission cell improved the detection limits (LOD) compared to the use of attenuated total reflectance measurements by a factor of approximately 80. Using the most appropriate experimental conditions for the CS 2 generation and LPME preconcentration, the precision of the methodology, expressed as the relative standard deviation (RSD), was of the order of 3.1% and the absolute LOD was 0.3 μg dithiocarbamate, which corresponds to 60–120 μg kg −1, for a sample mass ranging from 2.5 to 5 g. The usefulness of the methodology has been evidenced by the determination of mancozeb residues in strawberries, lettuce and corn samples at concentrations between 1 and 5 mg kg −1, where the VP-LPME IR provided results comparable with those obtained by a head space gas chromatography mass spectrometry reference procedure.