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Journal articles on the topic 'Pesticide residues in food – Testing – Methodology'

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Published: 4 June 2021
Last updated: 3 February 2022

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1

Mcmahon, Bernadette M., and Jerry A. Burke. "Expanding and Tracking the Capabilities of Pesticide Multiresidue Methodology Used in the Food and Drug Administration's Pesticide Monitoring Programs." Journal of AOAC INTERNATIONAL 70, no. 6 (November 1, 1987): 1072–81. http://dx.doi.org/10.1093/jaoac/70.6.1072.

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Abstract Foods analyzed for pesticide residues in the monitoring programs of the U.S. Food and Drug Administration (FDA) are most often examined by using one or more of the multiresidue methods developed for this purpose over the years. Because no single method can be used for all potential residues, each commodity is examined by a method or methods which will identify and/or determine the chemicals most likely to have been used. FDA conducts research to develop new multiresidue methods, which are included in monitoring programs as needed to cover additional chemicals. FDA's multiresidue methods have undergone continuous study over a 20 year period to ascertain which compounds can and cannot be recovered by them. FDA continues to perform tests to discover a compound's analytical characteristics. Protocols have been published to direct the testing of additional compounds so that new information can be added to the existing compilations. Methods capable of determining residues of single pesticides are used to analyze selected commodities for residues of high priority that cannot be determined by existing multiresidue methods. Pestrak, a computerized listing of pesticide analytical information, has been developed by FDA to keep track of the capabilities of multiresidue methods and the coverage of residues by the single residue methods used in FDA monitoring.
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2

Wilkowska, Angelika, and Marek Biziuk. "Determination of pesticide residues in food matrices using the QuEChERS methodology." Food Chemistry 125, no. 3 (April 2011): 803–12. http://dx.doi.org/10.1016/j.foodchem.2010.09.094.

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3

Beneito-Cambra, Miriam, Bienvenida Gilbert-López, David Moreno-González, Marcos Bouza, Joachim Franzke, Juan F. García-Reyes, and Antonio Molina-Díaz. "Ambient (desorption/ionization) mass spectrometry methods for pesticide testing in food: a review." Analytical Methods 12, no. 40 (2020): 4831–52. http://dx.doi.org/10.1039/d0ay01474e.

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4

SMITH, G. C., J. N. SOFOS, M. J. AARONSON, J. B. MORGAN, J. D. TATUM, and G. R. SCHMIDT. "INCIDENCE OF PESTICIDE RESIDUES AND RESIDUES OF CHEMICALS SPECIFIED FOR TESTING IN U.S. BEEF BY THE EUROPEAN COMMUNITY." Journal of Muscle Foods 5, no. 3 (September 1994): 271–84. http://dx.doi.org/10.1111/j.1745-4573.1994.tb00536.x.

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5

Schenck, Frank J., Roberta Wagner, Michael K. Hennessy, and Joseph L. Okrasinski. "Screening Procedure for Organochlorine and Organophosphorus Pesticide Residues in Eggs using a Solid-Phase Extraction Cleanup and Gas Chromatographic Detection." Journal of AOAC INTERNATIONAL 77, no. 4 (July 1, 1994): 1036–40. http://dx.doi.org/10.1093/jaoac/77.4.1036.

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Abstract A solid-phase extraction (SPE) screening procedure for the isolation and gas chromatographic (GC) determination of organochlorine and organophosphorus pesticide residues in eggs is described. Eggs are extracted with acetonitrile. The extract is subjected to a cleanup on tandem C18 and Florisil SPE columns. Organochlorine and organophosphorus pesticide residues are determined by GC with electron capture and flame photometric detection, respectively. Because the injected extracts are free from matrix interferences, the amount of residue present is easy to calculate. The average recoveries of 9 spiked organochlorine pesticide residues (0.01–1.0 ppm) ranged from 80.9 to 91.1 %. The average recoveries of 7 spiked organophosphorus pesticide residues (0.02–0.50 ppm) ranged from 80.3 to 89.5%. The SPE method results in a 90% reduction in organic solvent consumption and an 85% reduction in hazardous waste production compared with the AOAC methodology.
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6

Luke, Milton A., Herbert T. Masumoto, Thomas Cairns, and Harvey K. Hundley. "Levels and Incidences of Pesticide Residues in Various Foods and Animal Feeds Analyzed by the Luke Multiresidue Methodology for Fiscal Years 1982-1986." Journal of AOAC INTERNATIONAL 71, no. 2 (March 1, 1988): 415–33. http://dx.doi.org/10.1093/jaoac/71.2.415.

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Abstract During a 5 year period from 1982 to 1986, the FDA Los Angeles District Laboratory analyzed 19 851 samples of domestic and imported food and feed commodities for pesticide residues. A single, rapid, multiresidue method was used. The resultant data have been compiled showing the commodities sampled and the identity and range of levels of pesticide residues detected, including an indication of those residue findings that did not comply with U.S. federal tolerance levels. The residue data presented should not be viewed as being representative of the U.S. food supply; rather, the results are indicative of a surveillance- and compliance-oriented sampling of various food shipments collected by the Los Angeles District.
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7

Chang, Qiao-Ying, Guo-Fang Pang, Chun-Lin Fan, Hui Chen, Fang Yang, Jie Li, and Bi-Fang Wen. "High-Throughput Analytical Techniques for the Determination of the Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VII: A GC-MS, GC-MS/MS, and LC-MS/MS Study of the Degradation Profiles of Pesticide Residues in Green Tea." Journal of AOAC INTERNATIONAL 99, no. 6 (November 1, 2016): 1619–27. http://dx.doi.org/10.5740/jaoacint.16-0158.

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Abstract GC-MS, GC-tandem MS (MS/MS), and LC-MS/MS were used to mathematically define the degradation profiles of pesticide residues in two field trials. Nineteen pesticides were studied in the first field trial and 11 in the second. The results of the field trials demonstrated that the degradation profiles of pesticide residues in green tea can be described with power functions to successfully estimate the amount of time, following pesticide application, pesticide residues appearing in tea in concentrations at and/or above the maximum residue limit (MRL) decrease to concentrations below the MRL. Stability tests on green tea samples stored at room temperature were conducted to determine whether pesticide-incurred green tea samples prepared according to the method used in the field trials would be suitable for the preparation of reference standards for laboratory-proficiency testing trials. This paper reports the results of a GC-MS, GC-MS/MS, and LC-MS/MS study, as well as the suitability of the samples prepared under these conditions for use as pesticide reference standards in tea analysis.
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8

Zhang, Jing Jing, and Hong Yang. "Advance in Methodology and Strategies To Unveil Metabolic Mechanisms of Pesticide Residues in Food Crops." Journal of Agricultural and Food Chemistry 69, no. 9 (March 1, 2021): 2658–67. http://dx.doi.org/10.1021/acs.jafc.0c08122.

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9

Martnez Vidal, Jos Luis, Jos Luis Fernndez Moreno, Francisco Javier Arrebola Libanas, and Antonia Garrido Frenich. "Application of Low-Pressure Gas Chromatography/Tandem Mass Spectrometry to the Determination of Pesticide Residues in Tropical Fruits." Journal of AOAC INTERNATIONAL 90, no. 4 (July 1, 2007): 1146–64. http://dx.doi.org/10.1093/jaoac/90.4.1146.

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Abstract A multiresidue method has been developed for determining pesticide residues in the tropical fruits kiwi, custard apple, and mango. The intended purpose of the method is for regulatory analyses of commodities for pesticides that have established maximum residue limits. A fast and simple extraction method with cyclohexaneethyl acetate (1 + 1, v/v) and a high-speed homogenizer was optimized. Pressurized liquid extraction was evaluated as an alternative automated extraction technique. The pesticide residues were determined by using low-pressure gas chromatography coupled to tandem mass spectrometry. The proposed methodology was validated for each matrix. Pesticide recoveries ranged from 70 to 110%, with repeatability relative standard deviations of 18% at spiking levels of 12 and 50 g/kg. The limits of quantitation were in the range of 0.036.17 g/kg, and the limits of detection were between 0.01 and 3.75 g/kg. Mango can be selected as a representative matrix for calibration on the basis of the results of a potential matrix effect study. The method was successfully applied to the determination of pesticide residues in real samples in Spain.
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10

Ambrus, Árpád, Gregory Noonan, Anikó Németh, Gabriella Kötelesné-Suszter, Michelangelo Anastassiades, Kamirán Á. Hamow, and Etelka M. Solymosné. "Testing the Accuracy of Analytical Standard Solutions Used for Quantitative Determination of Pesticide Residues." Journal of AOAC INTERNATIONAL 100, no. 4 (July 1, 2017): 1058–61. http://dx.doi.org/10.5740/jaoacint.17-0018.

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11

Vongbuddhapitak, Amara, Kanokporn Atisook, Gobthong Thoophom, Boonpai Sungwaranond, Yuwadee Lertreungdej, Jitpaka Suntudrob, and Ladda Kaewklapanyachareon. "Dietary Exposure of Thais to Pesticides During 1989–1996." Journal of AOAC INTERNATIONAL 85, no. 1 (January 1, 2002): 134–40. http://dx.doi.org/10.1093/jaoac/85.1.134.

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Abstract To monitor the exposure of the Thai to pesticide residues in foods, the intake of pesticides based on the total diet approach has been studied in Thailand continually since 1989. Food items were chosen and their proportions of daily consumption were calculated from the national food consumption survey conducted by the Department of Health in 1986. Seventy-seven items of food including drinking water were classified into 12 groups according to their sources of contamination and the analytical methods used. Shopping lists and standard procedures for collecting samples and cooking were developed. Twelve food composites from each of the 4 regions were analyzed for nearly 100 pesticides. All analyses used multiresidue analytical methods, and the total daily dietary intakes of pesticide residues were estimated from the average amount of food consumed by Thais. Among 24 pesticides found in the 8 year study, DDT, dimethoate, methamidophos, and parathion methyl were found every year. However, dietary intakes of all pesticides were far below the established acceptable daily intake. In 1999, the study methodology was redesigned to accommodate the new national food consumption survey data.
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12

Tsagkaris, Aristeidis S., Jana Pulkrabova, and Jana Hajslova. "Optical Screening Methods for Pesticide Residue Detection in Food Matrices: Advances and Emerging Analytical Trends." Foods 10, no. 1 (January 5, 2021): 88. http://dx.doi.org/10.3390/foods10010088.

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Pesticides have been extensively used in agriculture to protect crops and enhance their yields, indicating the need to monitor for their toxic residues in foodstuff. To achieve that, chromatographic methods coupled to mass spectrometry is the common analytical approach, combining low limits of detection, wide linear ranges, and high accuracy. However, these methods are also quite expensive, time-consuming, and require highly skilled personnel, indicating the need to seek for alternatives providing simple, low-cost, rapid, and on-site results. In this study, we critically review the available screening methods for pesticide residues on the basis of optical detection during the period 2016–2020. Optical biosensors are commonly miniaturized analytical platforms introducing the point-of-care (POC) era in the field. Various optical detection principles have been utilized, namely, colorimetry, fluorescence (FL), surface plasmon resonance (SPR), and surface enhanced Raman spectroscopy (SERS). Nanomaterials can significantly enhance optical detection performance and handheld platforms, for example, handheld SERS devices can revolutionize testing. The hyphenation of optical assays to smartphones is also underlined as it enables unprecedented features such as one-click results using smartphone apps or online result communication. All in all, despite being in an early stage facing several challenges, i.e., long sample preparation protocols or interphone variation results, such POC diagnostics pave a new road into the food safety field in which analysis cost will be reduced and a more intensive testing will be achieved.
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13

Beceiro-González, Elisa, María J. González-Castro, Soledad Muniategui-Lorenzo, Purificación López-Mahía, and Darío Prada-Rodríguez. "Analytical Methodology for the Determination of Organochlorine Pesticides in Vegetation." Journal of AOAC INTERNATIONAL 95, no. 5 (September 1, 2012): 1291–310. http://dx.doi.org/10.5740/jaoacint.sge_beceiro-gonzalez.

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Abstract Due to the extensive use of organochlorine pesticides (OCPs) for agricultural purposes and their high persistence and low biodegradability, they have become an important group of contaminants. Detection and quantification of pesticide residues in food, particularly fruits and vegetables, is of growing concern for producers, consumers, and governments. The most widely used pretreatment for the extraction of pesticides in plants is based on solvent extraction liquid-solid extraction (LSE). LSE can be carried out using Soxhlet, shake-flask, homogenization, sonication, and, more recently, microwave-assisted extraction, pressurized liquid extraction, and supercritical fluid extraction. Furthermore, new analytical procedures using the extraction with sorbents, such as solid-phase micro-extraction, stir bar sorptive extraction, and matrix solid-phase dispersion, have also been used. On the other hand, a wide range of cleanup methods (liquid–liquid extraction, solid-phase extraction, gel permeation chromatography, and dispersive solid-phase extraction; and chromatographic techniques with electron capture detector and mass spectrometry detector; and HPLC with a ultraviolet detector are reported in the literature. This article reviews the applicability, advantages, and disadvantages of various sample preparation techniques (traditional and new techniques) for the analysis of OCPs in different plants and plant materials. It covers more than 15 years of published methods in which pesticide residues have been determined in a wide range of vegetation samples (fruits, horticultural samples, medicinal plants, tree leaves, etc.) by the use of chromatographic techniques after various sample preparation steps. A great number of applications in different plant material are provided. To the best of the authors' knowledge, previously published reviews have not covered as wide and exhaustive range of vegetation matrixes as presented here. A summary of pesticide levels cited in the literature is included.
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14

JONES, SHUNA A., ROBERT S. SALTER, TIM GOLDSMITH, JULIO QUINTANA, PAUL RAPNICKI, KAREN SHUCK, JIM E. WELLS, MARILYN J. SCHNEIDER, and DEE GRIFFIN. "Development and Model Testing of Antemortem Screening Methodology To Predict Required Drug Withholds in Heifers†." Journal of Food Protection 77, no. 2 (February 1, 2014): 292–98. http://dx.doi.org/10.4315/0362-028x.jfp-13-267.

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A simple, cow-side test for the presence of drug residues in live animal fluids would provide useful information for tissue drug residue avoidance programs. This work describes adaptation and evaluation of rapid screening tests to detect drug residues in serum and urine. Medicated heifers had urine, serum, and tissue biopsy samples taken while on drug treatment. Samples were tested by rapid methods and high-performance liquid chromatography (HPLC). The adapted microbial inhibition method, kidney inhibition swab test, was useful in detecting sulfadimethoxine in serum, and its response correlated with the prescribed withdrawal time for the drug, 5 to 6 days posttreatment. The lateral flow screening method for flunixin and beta-lactams, adapted for urine, was useful in predicting flunixin in liver detected by HPLC, 96 h posttreatment. The same adapted methods were not useful to detect ceftiofur in serum or urine due to a lack of sensitivity at the levels of interest. These antemortem screening test studies demonstrated that the method selected, and the sampling matrix chosen (urine or serum), will depend on the drug used and should be based on animal treatment history if available. The live animal tests demonstrated the potential for verification that an individual animal is free of drug residues before sale for human consumption.
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15

Jeong, In-Seek, Byung-Man Kwak, Jang-Hyuk Ahn, and Seung-Hwan Jeong. "Determination of pesticide residues in milk using a QuEChERS-based method developed by response surface methodology." Food Chemistry 133, no. 2 (July 2012): 473–81. http://dx.doi.org/10.1016/j.foodchem.2012.01.004.

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16

Fehringer, Norbert V., and Stephen M. Walters. "Evaluation of Capillary Gas Chromatography for Pesticide and Industrial Chemical Residue Analysis. II. Comparison of Quantitative Results Obtained on Capillary and Packed Columns." Journal of AOAC INTERNATIONAL 69, no. 1 (January 1, 1986): 90–93. http://dx.doi.org/10.1093/jaoac/69.1.90.

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Abstract Results of pesticide and industrial chemical residue determinations, using both capillary and packed column gas chromatography (GC), in 3 Food and Drug Administration (FDA) laboratories have been compiled and compared. Samples consisted of food products collected for routine residue screening by the respective laboratories. Extracts were prepared by conventional multiresidue methodology. Capillary column systems and operating conditions were selected at the discretion of each laboratory and were therefore variable, although split/splitless injectors in the split mode were used with prescribed precautions in all cases. Packed column systems were operated as specified in the FDA Pesticide Analytical Manual (PAM). Overall correlation between the 2 systems, expressed as the average ratio of packed column result to capillary column result, was 0.99 for 120 determinations in 41 samples. The higher resolving power of the capillary systems allowed quantitation of several residues that were incompletely separated and therefore unquantifiable using the packed columns. Capillary column GC with the split injection technique, used with appropriate precautions, was found to be both reliable and advantageous for regulatory determination of pesticide and industrial chemical residues in foods and feeds.
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17

Schenck, Frank J. "Screening of Nonfatty Fish for Organochlorine Pesticide Residues by Solid-Phase Extraction Cleanup: Interlaboratory Study." Journal of AOAC INTERNATIONAL 79, no. 5 (September 1, 1996): 1215–19. http://dx.doi.org/10.1093/jaoac/79.5.1215.

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Abstract Six U.S. Food and Drug Administration laboratories participated in an interlaboratory trial of a solidphase extraction cleanup method for determination of pesticides in nonfatty seafood products. The participants analyzed control and fortified (about 0.050 ppm lindane, heptachlor epoxide, p,p′-DDE, and endrin) croaker and flounder samples and a sea trout sample containing incurred p,p′-DDE residues. Mean recoveries of the fortified residues from the fish ranged from 89.1 to 107.8%. The within-laboratory coefficients of variation (CVs) ranged from 4.2 to 8.5%, and the among-laboratory CVs ranged from 10.9 to 26.5%. The 6 laboratories reported a mean value of 0.040 ppm p,p′-DDE in a fish sample which contained incurred residues. The same value (0.040 ppm) was obtained by using official methodology. The within-laboratory CVs ranged from 3.5 to 18.3%, and the among-laboratory CV was 17.3%.
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18

Hopper, Marvin L. "Extraction and Cleanup of Organochlorine and Organophosphorus Pesticide Residues in Fats by Supercritical Fluid Techniques." Journal of AOAC INTERNATIONAL 80, no. 3 (May 1, 1997): 639–46. http://dx.doi.org/10.1093/jaoac/80.3.639.

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Abstract A supercritical fluid extraction and cleanup procedure was developed for separating organochlorine and organophosphorus pesticides from fats. Supercritical carbon dioxide modified with 3% (v/v) acetonitrile was used to extract the pesticides at 6O°C and separate the pesticides from the fats at 4000 psi and 95°C on an in-line C? silica-based column. The extraction and cleanup procedure gave good recoveries for 43 of 62 nonpolar to moderately polar organochlorine and organophosphorus pesticides from fats, whereas 49 were recovered through conventional Florisil column cleanup before quantitation. This procedure can extract and clean up pesticide residues from 0.65 g animalbased fat and 1.0 g oils. Coeluted residues in the pesticide fraction ranged from 2.5 mg for butterfat to 0.8 mg for corn oil. Results for samples analyzed with this integrated extraction cleanup procedure were reproducible and comparable with results obtained with the current Total Diet Study methodology.
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19

Goodman, Julie E., Robyn L. Prueitt, Paolo Boffetta, Crispin Halsall, and Andrew Sweetman. "“Good Epidemiology Practice” Guidelines for Pesticide Exposure Assessment." International Journal of Environmental Research and Public Health 17, no. 14 (July 15, 2020): 5114. http://dx.doi.org/10.3390/ijerph17145114.

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Both toxicology and epidemiology are used to inform hazard and risk assessment in regulatory settings, particularly for pesticides. While toxicology studies involve controlled, quantifiable exposures that are often administered according to standardized protocols, estimating exposure in observational epidemiology studies is challenging, and there is no established guidance for doing so. However, there are several frameworks for evaluating the quality of published epidemiology studies. We previously developed a preliminary list of methodology and reporting standards for epidemiology studies, called Good Epidemiology Practice (GEP) guidelines, based on a critical review of standardized toxicology protocols and available frameworks for evaluating epidemiology study quality. We determined that exposure characterization is one of the most critical areas for which standards are needed. Here, we propose GEP guidelines for pesticide exposure assessment based on the source of exposure data (i.e., biomonitoring and environmental samples, questionnaire/interview/expert record review, and dietary exposures based on measurements of residues in food and food consumption). It is expected that these GEP guidelines will facilitate the conduct of higher-quality epidemiology studies that can be used as a basis for more scientifically sound regulatory risk assessment and policy making.
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20

Liu, Guangyang, Meng Lu, Xiaodong Huang, Tengfei Li, and Donghui Xu. "Application of Gold-Nanoparticle Colorimetric Sensing to Rapid Food Safety Screening." Sensors 18, no. 12 (November 27, 2018): 4166. http://dx.doi.org/10.3390/s18124166.

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Due to their unique optical properties, narrow size distributions, and good biological affinity, gold nanoparticles have been widely applied in sensing analysis, catalytic, environmental monitoring, and disease therapy. The color of a gold nanoparticle solution and its maximum characteristic absorption wavelength will change with the particle size and inter-particle spacing. These properties are often used in the detection of hazardous chemicals, such as pesticide residues, heavy metals, banned additives, and biotoxins, in food. Because the gold nanoparticles-colorimetric sensing strategy is simple, quick, and sensitive, this method has extensive applications in real-time on-site monitoring and rapid testing of food quality and safety. Herein, we review the preparation methods, functional modification, photochemical properties, and applications of gold nanoparticle sensors in rapid testing. In addition, we elaborate on the colorimetric sensing mechanisms. Finally, we discuss the advantages and disadvantages of colorimetric sensors based on gold nanoparticles, and directions for future development.
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21

Tolcha, Teshome, Tura Gemechu, Said Al-Hamimi, Negussie Megersa, and Charlotta Turner. "High Density Supercritical Carbon Dioxide for the Extraction of Pesticide Residues in Onion with Multivariate Response Surface Methodology." Molecules 25, no. 4 (February 24, 2020): 1012. http://dx.doi.org/10.3390/molecules25041012.

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The excessive use of pesticides is a serious health problem due to their toxicity and bioaccumulation through the food chain. Due to the complexity of foods, the analysis of pesticides is challenging often giving large matrix effects and co-extracted compounds. To overcome this problem, a selective and “green” supercritical fluid extraction method was developed, using neat carbon dioxide as a solvent at pressures of up to 800 bars. A Box–Behnken response surface experimental design was used, with the independent variables of density (0.70−1.0 g mL−1), temperature (40−70 °C), and volume (10−40 mL) of solvent, and the dependent variable of extracted amount of pesticides. The optimum extraction condition was found at the use of 29 mL of supercritical CO2 at 0.90 g mL−1 and 53 °C (corresponding to 372 bars of pressure). It was observed that increasing the density of CO2 significantly increased the extraction recovery of endrin and 2,4′-dichlorodiphenyldichloroethane. Matrix-matched calibration curves showed satisfactory linearity (R2 ≥ 0.994), and LODs ranged from 0.2 to 2.0 ng g−1. Precision was lower than 11% and recoveries between 80%–103%. Thus, the developed method could efficiently be used for trace analysis of pesticides in complex food matrices without the use of organic solvents.
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22

Cherukuri, Sreenivasa Rao, V. Shashi Bhushan, A. Harinatha Reddy, D. Ravindranath, M. Aruna, S. Swarupa Rani, B. Ramesh, and M. Hymavathy. "Method Validation for Qualitative and Quantitative Analysis of Pesticide Residues in Tomato with GC-MS/MS (TQD) for Food Safety Testing." International Journal of Agriculture, Environment and Biotechnology 8, no. 2 (2015): 457. http://dx.doi.org/10.5958/2230-732x.2015.00053.4.

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23

Martínez Vidal, Jose L., Manuel J. González-Rodríguez, Francisco J. Arrebola, Antonia Garrido Frenich, Francisco J. Sánchez López, and Nielene Mora Díez. "Selective Extraction and Determination of Multiclass Pesticide Residues in Post-Harvest French Beans by Low-Pressure Gas Chromatography/Tandem Mass Spectrometry." Journal of AOAC INTERNATIONAL 86, no. 4 (July 1, 2003): 856–67. http://dx.doi.org/10.1093/jaoac/86.4.856.

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Abstract A selective and reliable extraction procedure was developed and validated to determine multiclass pesticide residues in lyophilized agricultural plants by low-pressure gas chromatography coupled with tandem mass spectrometry. The method is based on a rapid and simple extraction of the lyophilized sample with dichloromethane. The results were compared with those obtained by using fresh and naturally dried samples. Slightly better recoveries and precision values were obtained for the lyophilized samples. The application of the proposed methodology was tested by analyzing French bean plants from an agricultural area of Almería (Spain). The availability of this methodology, which is capable of detecting a high number of analytes in a single analysis, has priority in analyses for a large number of pesticides used on individual commodities.
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24

Abdulra'uf, Lukman Bola, Ala Yahya Sirhan, and Guan Huat Tan. "Applications of Experimental Design to the Optimization of Microextraction Sample Preparation Parameters for the Analysis of Pesticide Residues in Fruits and Vegetables." Journal of AOAC INTERNATIONAL 98, no. 5 (September 1, 2015): 1171–85. http://dx.doi.org/10.5740/jaoacint.sge3abdulrauf.

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Abstract Sample preparation has been identified as the most important step in analytical chemistry and has been tagged as the bottleneck of analytical methodology. The current trend is aimed at developing cost-effective, miniaturized, simplified, and environmentally friendly sample preparation techniques. The fundamentals and applications of multivariate statistical techniques for the optimization of microextraction sample preparation and chromatographic analysis of pesticide residues are described in this review. The use of Placket-Burman, Doehlert matrix, and Box-Behnken designs are discussed. As observed in this review, a number of analytical chemists have combined chemometrics and microextraction techniques, which has helped to streamline sample preparation and improve sample throughput.
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da Silva Sousa, Jonas, Rubens Carius de Castro, Gilliane de Albuquerque Andrade, Cleidiane Gomes Lima, Lucélia Kátia Lima, Maria Aparecida Liberato Milhome, and Ronaldo Ferreira do Nascimento. "Evaluation of an analytical methodology using QuEChERS and GC-SQ/MS for the investigation of the level of pesticide residues in Brazilian melons." Food Chemistry 141, no. 3 (December 2013): 2675–81. http://dx.doi.org/10.1016/j.foodchem.2013.05.027.

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26

Young, Susan J. V., Charles H. Parfitt, Richard F. Newell, and Terry D. Spittler. "Homogeneity of Fruits and Vegetables Comminuted in a Vertical Cutter Mixer." Journal of AOAC INTERNATIONAL 79, no. 4 (July 1, 1996): 976–80. http://dx.doi.org/10.1093/jaoac/79.4.976.

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Abstract The homogeneity of comminuted composites of 20 lb samples of apples, cabbage, and green beans containing field-incurred residues of p,p′-methoxychlor was studied to determine whether a 5 min comminution in a 40 qt vertical cutter mixer produces a homogeneous composite and whether the size of test portions used accurately represents the composite. Duplicate test portions of 100,50,25, 10,5, and 2 g taken from each of 6 separate sections of the mixer were analyzed by standard pesticide residue methodology for p,p′-methoxychlor. Results of this study confirmed that comminution of fresh produce in a 40 qt vertical cutter mixer, according to instructions described in the U.S. Food and Drug Administration's Pesticide Analytical Manual, Volume 1, section 203B, produces a homogeneous composite. No significant differences were found in the data for the 3 crops taken from the 6 sections of the mixer. Test portion weights of 100, 50, and 25 g produced equivalent results for all 3 crops. Statistically significant differences were observed for cabbage at 2,5, and 10 g and for green beans at 2 g.
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27

Key, Pauline E., Alan L. Patey, Simon Rowling, Anne Wilbourn, and Fiona M. Worner. "International Proficiency Testing of Analytical Laboratories for Foods and Feeds from 1990 to 1996: The Experiences of the United Kingdom Food Analysis Performance Assessment Scheme." Journal of AOAC INTERNATIONAL 80, no. 4 (July 1, 1997): 895–900. http://dx.doi.org/10.1093/jaoac/80.4.895.

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Abstract The Food Analysis Performance Assessment Scheme (FAPAS) organized by a Secretariat of the UK Ministry of Agriculture, Fisheries, and Food has checked the proficiency of analytical laboratories for foods and feeds from 1990 to 1996. FAPAS was started for UK laboratories but was expanded worldwide at the request of analysts in other countries who did not have a home-based scheme. Thirteen thousand homogeneity-checked test materials were issued, covering a very wide range of analytes, including pesticides, toxins, veterinary drug residues, trace and nutritional elements, food colors, preservatives, sweeteners, alcohol congeners, fatty acids, nitrate, and proximate analysis. Participants returned 85% of requested data, and 47 000 z- score proficiency assessments were made, of which 81% were satisfactory. Evidence is presented of improvements in overall analytical ability with increased participation in proficiency testing in the areas of proximate analysis; organochlorine pesticide analysis; and lead, mercury, and acesul- fame-K analyses. Little improvement was shown in other analytical areas such as calcium analysis. Overall accuracies for analysis of specific pesticides and specific trace elements in the circulated test materials were compared.
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Sumiati, Astri, and Reza Prakoso Dwi Julianto. "ANALISIS RESIDU PESTISIDA PADA JERUK MANIS DI KECAMATAN DAU, MALANG." BUANA SAINS 17, no. 1 (July 24, 2017): 19. http://dx.doi.org/10.33366/bs.v17i1.574.

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Citrus is one type of fruit that is highly favored by the people. Citrus plants are vulnerable to pests and plant diseases that intensive use of pesticides in the field can not be avoided. Citrus fruits commonly consumed in the form of raw materials that need to be considered food quality and safety of citrus fruits to public health. This study aims to identify and analyze pesticide residues in citrus fruits in the district of Dau, Malang (a case study in the Village Tegalwaru subdistrict Dau, Malang) as one of the centers of citrus production in East Java with the use of pesticides are quite diverse. This research is a survey and observational with cross sectional approach. Data use of pesticides by farmers was measured by a survey conducted for the farmers and merchants. The sample was 3 kg of oranges produced by three farmers and 3 kg of oranges produced by 3 merchants Village Tegalwaru District of Dau, Malang where interviews illustrate the differences in the type and frequency of the use of pesticides during the growing season oranges, which is a high level (sample A ), medium (sample B) and low (sample C). The measurement results residues acephate, carbofuran, carbosulfan, diazinon, dimethomorp, fenobucarb, profenofos, pyrethrin everything is still below the Limit of Detection (LOD) testing in the laboratory PT. Angler Biochem Lab. In profenofos residue tests on samples found to be higher farmer is 0.108 ppm compared with a sample of traders is 0,050 ppm. The conclusions of this study are bauh oranges produced by farmers in the sub-district Tegalwaru Dau, Malang get evidence that pesticide residues are still below the prescribed MRL.
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TIAN, YA-YA, SI MI, YA-XIN SANG, CHUN-YU KANG, and XIANG-HONG WANG. "Ozone Degradation of Prometryn in Ruditapes philippinarum: Response Surface Methodology Optimization and Toxicity Assessment." Journal of Food Protection 83, no. 9 (May 7, 2020): 1641–48. http://dx.doi.org/10.4315/jfp-20-076.

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ABSTRACT This study optimized the method for ozone (O3) degradation of prometryn in the clam Ruditapes philippinarum and evaluated toxicity changes during ozone degradation. The gas chromatography method for the detection of prometryn was appropriately improved. The linear range was 5 to 500 ng/mL, with a correlation coefficient of 0.9964. The addition concentration of prometryn was 0.025 to 0.100 mg/kg, the recovery was 77.97 to 85.00%, the relative standard deviation (n = 6) was 2.36 to 7.86%, and the limit of detection was 0.3 μg/kg. Using the central composite design in two experiments, ozone as gas and ozone dissolved in water, the effect of degradation rate was studied on three variables: ozone concentration, temperature, and exposure time. Ozone as gas and ozone dissolved in water have the same degradation effect on prometryn. The O3 concentration was 4.2 mg/L, the temperature was 40°C, the exposure time was 10 min, and the maximum degradation rate was 89.94 and 89.69% for the two experiments, respectively. In addition, the toxicity of ozone degradation products was evaluated using buffalo rat liver cells. After ozone treatment for 30 min, the toxicity of the ozone degradation products was reduced to 52.15% compared with that of prometryn itself. The toxicity of the ozone degradation products increased slightly when the ozonation time was prolonged; the toxicity at 180 min was greater than that of the parent compound prometryn. Overall, the application of ozone degradation of pesticide residues is a promising new technology. This study determined better degradation conditions for prometryn in R. philippinarum and also provided a theoretical basis for the widespread use of ozone technology in the future. HIGHLIGHTS
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Vicini, John L., William R. Reeves, John T. Swarthout, and Katherine A. Karberg. "Glyphosate in livestock: feed residues and animal health1." Journal of Animal Science 97, no. 11 (September 9, 2019): 4509–18. http://dx.doi.org/10.1093/jas/skz295.

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Abstract Glyphosate is a nonselective systemic herbicide used in agriculture since 1974. It inhibits 5-enolpyruvylshikimate-3-phosphate (EPSP) synthase, an enzyme in the shikimate pathway present in cells of plants and some microorganisms but not human or other animal cells. Glyphosate-tolerant crops have been commercialized for more than 20 yr using a transgene from a resistant bacterial EPSP synthase that renders the crops insensitive to glyphosate. Much of the forage or grain from these crops are consumed by farm animals. Glyphosate protects crop yields, lowers the cost of feed production, and reduces CO2 emissions attributable to agriculture by reducing tillage and fuel usage. Despite these benefits and even though global regulatory agencies continue to reaffirm its safety, the public hears conflicting information about glyphosate's safety. The U.S. Environmental Protection Agency determines for every agricultural chemical a maximum daily allowable human exposure (called the reference dose, RfD). The RfD is based on amounts that are 1/100th (for sensitive populations) to 1/1,000th (for children) the no observed adverse effects level (NOAEL) identified through a comprehensive battery of animal toxicology studies. Recent surveys for residues have indicated that amounts of glyphosate in food/feed are at or below established tolerances and actual intakes for humans or livestock are much lower than these conservative exposure limits. While the EPSP synthase of some bacteria is sensitive to glyphosate, in vivo or in vitro dynamic culture systems with mixed bacteria and media that resembles rumen digesta have not demonstrated an impact on microbial function from adding glyphosate. Moreover, one chemical characteristic of glyphosate cited as a reason for concern is that it is a tridentate chelating ligand for divalent and trivalent metals; however, other more potent chelators are ubiquitous in livestock diets, such as certain amino acids. Regulatory testing identifies potential hazards, but risks of these hazards need to be evaluated in the context of realistic exposures and conditions. Conclusions about safety should be based on empirical results within the limitations of model systems or experimental design. This review summarizes how pesticide residues, particularly glyphosate, in food and feed are quantified, and how their safety is determined by regulatory agencies to establish safe use levels.
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ZENG, S. S., S. HART, E. N. ESCOBAR, and K. TESFAI. "Validation of Antibiotic Residue Tests for Dairy Goats." Journal of Food Protection 61, no. 3 (March 1, 1998): 344–49. http://dx.doi.org/10.4315/0362-028x-61.3.344.

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The SNAP test, LacTek test (B-L and CEF), Charm Bacillus sterothermophilus var. calidolactis disk assay (BsDA), and Charm II Tablet Beta-lactam sequential test were validated using antibiotic-fortified and -incurred goat milk following the protocol for test kit validations of the U.S. Food and Drug Administration Center for Veterinary Medicine. SNAP, Charm BsDA, and Charm II Tablet Sequential tests were sensitive and reliable in detecting antibiotic residues in goat milk. All three assays showed greater than 90% sensitivity and specificity at tolerance and detection levels. However, caution should be taken in interpreting test results at detection levels. Because of the high sensitivity of these three tests, false-violative results could be obtained in goat milk containing antibiotic residues below the tolerance level. Goat milk testing positive by these tests must be confirmed using a more sophisticated methodology, such as high-performance liquid chromatography, before the milk is condemned. LacTek B-L test did not detect several antibiotics, including penicillin G, in goat milk at tolerance levels. However, LacTek CEF was excellent in detecting ceftiofur residue in goat milk.
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Georgakopoulos, Panagiotis, Rodanthi Zachari, Marios Mataragas, Panagiotis Athanasopoulos, Eleftherios H. Drosinos, and Panagiotis N. Skandamis. "Optimisation of octadecyl (C18) sorbent amount in QuEChERS analytical method for the accurate organophosphorus pesticide residues determination in low-fatty baby foods with response surface methodology." Food Chemistry 128, no. 2 (September 2011): 536–42. http://dx.doi.org/10.1016/j.foodchem.2011.03.042.

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Shah, Syeda Kokab, Syeda Faryal Israr, Asif Khan Khatak, Abeer Kazmi, Amir Ali, Sher Mohammad, and Muhammad Irfan. "Quantitative analysis of fresh tomatoes (Solanum lycopersicum) for trace of pesticide residues from markets in Peshawar, Pakistan, using High Performance Thin Liquid Chromatography technique." Science and Technology Development Journal 23, no. 3 (September 30, 2020): 708–14. http://dx.doi.org/10.32508/stdj.v23i3.2470.

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Background: Vegetables and fruits are vital constituents of human diet, as it provides necessary minerals and nutrients to human body to carry out biological reactions and provide protection against various diseases and injuries. Solanum lycopersicum (tomato) is consider as cash crop in Asian countries and are fine source of vitamin C, potassium, folate, vitamin K, and other bioactive compounds including, phenolics, flavonoids, carotenoids, and alkaloids. Similar to other crops, tomato quality and yield is also affected by pests. Globally, approximately 37.8% of tomato yield is spoiled due to pests. To maintain the vegetable quality and attain more yield, pest management approaches are applied, though extensive use of toxic pesticides are becoming a part of our food chain and causing adverse effects. Methodology: The present research is intended to evaluate the levels of toxic pesticides in different tomato varieties collected from four vegetable markets (Hayatabad Phase 1, Chargano Chowk, Kohat Road and Tarnab farm) in Peshawar, Pakistan. After collection of tomato samples, level of pesticide residues (Cyhalothrin, Cypermethrin, Chlorpyrifos, Bifenthrin, and Imidacloprid) were detected using high performance thin liquid Chromatography (HPTLC). Results: After detection, level of pesticides in sample was compared with Maximum residue levels (MRLs). The magnitude of pesticides in samples was lesser to the Maximum residue levels (MRLs) provided by United State Drug Agency (USDA), though the quantity of Lambda Cyhalothrin present in the sample was almost equal to MRL (0.097 mg/kg). Conclusion: HPTLC is an efficient approach to detect pesticide traces in fruits and vegetables. Research work should be focused on it, to identify and control farmer practices which are highly linked to pesticide contamination in tomatoes and use of biopesticides should be encouraged. The cultivation of transgenic tomatoes can also be an efficient approach to elude the utilization of toxic pesticides.
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Otake, Takamitsu, Takashi Yarita, Tomoko Sakamoto, Masahiko Numata, and Akiko Takatsu. "Proficiency Testing for Quantification of Pesticide Residues in Treated Brown Rice Samples: Comparison of Performance of Japanese Official Multiresidue, Modified QuEChERS, and QuEChERS Methods." Journal of AOAC INTERNATIONAL 99, no. 3 (May 1, 2016): 821–29. http://dx.doi.org/10.5740/jaoacint.16-0038.

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Abstract To support analytical skill development, testing of proficiency in pesticide residue analysis in brown rice was conducted for 86 participating Japanese laboratories. Brown rice test samples containing three target pesticides (etofenprox, fenitrothion, and thiamethoxam) were distributed to participants who were free to choose an appropriate analytical method. Reported results were evaluated using a z-score based on the consensus values calculated from the participant analytical results and a z-score based on the high-reliability reference values determined by the National Metrology Institute of Japan (NMIJ). It was found that 80–89 and 82–85% of participants achieved acceptable consensus-value-based and NMIJ-reference-value-based z-scores, respectively. More than 80% of participants reported results obtained using the Japanese official multiresidue method, solid-phase extraction technique with the Quick, Easy, Cheap, Effective, Rugged, and Safe (modified QuEChERS) method or QuEChERS method. We show that the concentrations determined by the NMIJ using these three methods combined with isotope-dilution MS having high reliability agreed well and that the method performances were comparable.
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Romero-González, Roberto, Francisco Javier Arrebola Liébanas, Rosalía López-Ruiz, and Antonia Garrido Frenich. "Sample Treatment in Pesticide Residue Determination in Food by High-Resolution Mass Spectrometry: Are Generic Extraction Methods the End of the Road?" Journal of AOAC INTERNATIONAL 99, no. 6 (November 1, 2016): 1395–402. http://dx.doi.org/10.5740/jaoacint.16-0273.

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Abstract The use of high-resolution MS (HRMS) is becoming popular in laboratories for the determination of pesticide residues in food commodities. The recent improvements in the instrumentation have helped to increase the number of active compounds and transformation products that can be monitored within a simple chromatographic run. However, prior to instrumental determination, it is necessary to perform a nonspecific, or generic, sample treatment that allows the efficient extraction of several compounds with very relevant differences in their physical and chemical properties. In this sense, the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and its several modifications and the “dilute-and-shoot” extraction methodology have already revealed an enormous potential for their use together with chromatographic techniques coupled to HRMS. The potentiality and limitations of such a methodological combination have been evaluated in terms of sensitivity and selectivity when they are applied to the analysis of complex food matrixes. An evaluation of the scope of the methods, in terms of efficiency of the extraction and ionization steps, as well as the matrix effect, has also been carried out. Different solutions for the matrix effect have been considered, including improvement in clean-up steps, sample dilution, and matrix compensation by matrix-matched calibration or by the use of isotopically labeled standards.
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KOLAKOWSKI, BEATA M., KRYSTYNA JOHANIUK, HELEN ZHANG, and ETSUKO YAMAMOTO. "Analysis of Microbiological and Chemical Hazards in Edible Insects Available to Canadian Consumers." Journal of Food Protection 84, no. 9 (May 6, 2021): 1575–81. http://dx.doi.org/10.4315/jfp-21-099.

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ABSTRACT Edible insects are a novel food in most countries; their popularity is growing because of their high-protein and low-fat content, ease of cultivation, and small environmental impact. To our knowledge, this is the first report that addresses both microbiological and chemical hazards in edible insects. Samples were collected from retail stores or purchase through e-commerce. A total of 51 samples of dried whole insects or insect powder were tested for Escherichia coli, which serves as an indicator of the overall sanitation conditions throughout the food production chain, and the bacterial pathogen Salmonella spp. Neither Salmonella spp. nor E. coli (>100 CFU/g) was found in the samples analyzed. A total of 43 samples of crickets (protein bars, powders, flour, and whole insects) and 4 samples of silkworm (whole insects) were analyzed for up to 511 pesticides. Of these, 39 samples contained up to four pesticides; 34 samples were compliant and 5 samples were noncompliant with Canadian regulations. Seven pesticide residues were detected, with glyphosate and its metabolite, aminomethylphosphonic acid, as the predominant residues. Nineteen of the samples tested for pesticides were also analyzed for arsenic, cadmium, mercury, and lead; there was insufficient material remaining to allow testing of pesticides and metals. The positive rates for arsenic, cadmium, lead, and mercury were 100, 79, 58, and 74%, respectively. The detected concentrations ranged from 0.030 to 0.34 mg/kg for arsenic, from 0.031 to 0.23 mg/kg for cadmium, 0.019 to 0.059 mg/kg for lead, and from 0.94 to 28 μg/kg for mercury. Based on the lack of detection of microbiological contamination, and the positive rates and levels of pesticides and metals observed in the products, Health Canada determined that all insect products analyzed were safe for human consumption. This is a limited study; the Canadian Food Inspection Agency will continue to monitor this novel food. HIGHLIGHTS
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Abdulra'uf, Lukman Bola, and Guan Huat Tan. "Chemometric Study and Optimization of Headspace Solid-Phase Microextraction Parameters for the Determination of Multiclass Pesticide Residues in Processed Cocoa from Nigeria Using Gas Chromatography/Mass Spectrometry." Journal of AOAC INTERNATIONAL 97, no. 4 (July 1, 2014): 1007–11. http://dx.doi.org/10.5740/jaoacint.sgeabdulrauf.

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Abstract Solid-phase microextraction (SPME) is a solventless sample preparation method that combines sample preparation, isolation, concentration, and enrichment into one step. A simple and effective method coupling headspace-SPME to GC/MS was developed for the analysis of chlorpyrifos, fenitrothion, endosulfan I, and endosulfan II pesticide residues in cocoa powder. In this study, multivariate strategy was used to determine the significance of the factors affecting the SPME of the pesticides using a Plackett-Burman design, and the significant factors were optimized using central composite design. The analytes were extracted with 100 μm polydimethylsiloxane fibers according to the factorial design matrix and desorbed into a GC/MS instrument. The developed method was applied for the analysis of a cocoa powder sample, and it exhibited good figures of merit for the analytical methodology. Using the optimized conditions, the linearity ranged from 2.5 to 500 μg/kg (R2 > 0.99) using an internal standard calibration method, and the average recoveries were between 75 and 95%, with RSD values between 3.8 and 9.7%.
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Goon, Arnab, Raviraj Shinde, Bappa Ghosh, and Kaushik Banerjee. "Application of Automated Mini–Solid-Phase Extraction Cleanup for the Analysis of Pesticides in Complex Spice Matrixes by GC-MS/MS." Journal of AOAC INTERNATIONAL 103, no. 1 (January 1, 2020): 40–45. http://dx.doi.org/10.5740/jaoacint.19-0202.

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Abstract Background: Pesticide residues are routinely tested in spices for trade compliance. This results in a huge sample load for food testing laboratories and demands automation in sample preparation. Although there exists a method for the analysis of pesticides in fruits using an automated sample cleanup by mini–solid-phase extraction (mini-SPE) technique, no study is available to date on spices. Objective: This study aims to develop an automated sample cleanup method using mini-SPE technique in a range of spices, including chili powder, turmeric, black pepper, cumin, coriander, and cardamom. Methods: This automated sample preparation workflow involved an X-Y-Z instrument autosampler, and a set of mini-SPE cartridges comprising cleanup sorbents. Spice samples were extracted by acetonitrile, and the extract was put into an autosampler vial for automated mini-SPE cleanup before analysis by GC tandem MS. For an efficient cleanup, three different sorbent compositions were compared along with various automated workflows. Results: For the relatively simple matrixes (e.g., coriander, cumin, and cardamom), the LOQ for the target pesticides was 10 ng/g with acceptable recovery, and precision. The method provided an LOQ of 10 ng/g for around 77% of the compounds in the relatively complex matrixes (e.g., turmeric, chili powder, and black pepper). The remainder of the compounds had satisfactory recoveries at 20 ng/g and higher levels. Conclusions: Given its time effectiveness and efficient analytical performance, this method can be adopted in commercial food testing laboratories for time-bound analysis of a large volume of samples. Highlights: The study describes effectiveness of the automated mini-SPE cleanup in multiresidue analysis of pesticides in a range of spice matrixes. The method facilitates high-throughput residue analysis in compliance with the regulatory requirements of sensitivity and method performance.
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Verdon, Eric, Pierric Couëdor, Pierre Maris, Michel Laurentie, P. Batjoens, B. Brady, C. Branzell, et al. "Liquid Chromatographic Determination of Ampicillin Residues in Porcine Muscle Tissue by a Multipenicillin Analytical Method: European Collaborative Study." Journal of AOAC INTERNATIONAL 85, no. 4 (July 1, 2002): 889–900. http://dx.doi.org/10.1093/jaoac/85.4.889.

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Abstract A collaborative study involving 14 laboratories was conducted to determine residues of ampicillin in porcine muscle tissue by using a liquid chromatographic method developed for multipenicillin analysis that can quantitate 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer, pH 9, followed cleanup and concentration on a C18 solid-phase extraction column and reaction with benzoic anhydride at 50°C and with 1,2,4-triazole and mercury(II) chloride solution, pH 9.0, at 65°C. The derivatized compounds are eluted isocratically on a C8 column with a mobile phase of acetonitrile and phosphate buffer (pH 6; 0.1M) containing sodium thiosulfate and the ion-pair reagent tetrabutylammonium hydrogen sulfate. The penicillins are detected by UV absorption at 325 nm. The limit of detection and the limit of determination (quantitation) of the method were calculated to be approximately 3–5 and 25 μg/kg, respectively, in accordance with the criteria of European Union (EU) Decision No. 93/256/EEC. In this first interlaboratory study, collaborators were instructed to monitor 4 different penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, and amoxicillin) by analyzing 8 blind samples of muscle tissue in triplicate. These samples were prepared from 2 materials containing different concentrations of incurred ampicillin (63.5 μg/kg for material No. 1 and 358.1 μg/kg for material No. 2) and 1 blank material. The repeatability relative standard deviation and the reproducibility relative standard deviation were 10.2 and 17.4%, respectively, for material No. 1 and 7.0 and 16.0%, respectively, for material No. 2. These results demonstrate that the method is suitable for the determination of ampicillin residues in muscle tissue at the EU maximum residue limit (50 μg/kg) and above. However, the identification of positives by this procedure may need additional confirmation by techniques with greater specificity, such as liquid chromatography combined with mass spectrometry, or tandem mass spectrometry. Investigations regarding the basis of interlaboratory testing studies will further demonstrate the suitability of multiresidue methodology for detecting and quantitating other compounds in the family of penicillin antibiotics.
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Pang, Guo-Fang, Chun-Lin Fan, Yan-Zhong Cao, Fang Yan, Yan Li, Jian Kang, Hui Chen, et al. "High Throughput Analytical Techniques for the Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea by GC/MS, GC/MS/MS, and LC/MS/MS: Collaborative Study, First Action 2014.09." Journal of AOAC INTERNATIONAL 98, no. 5 (September 1, 2015): 1428–54. http://dx.doi.org/10.5740/jaoacint.15021.

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Abstract Thirty laboratories from fom North and South America, Europe, and Asia participated in this AOAC collaborative study (15 from China; five from Germany; two each from Italy and the United States; and one each from the Republic of Korea, Canada, Spain, Japan, Belgium, and India). Participants represented government regulatory, commercial testing, university, research institute, and private laboratories. The single-laboratory validated (SLV) tea method was evaluated in the collaborative study to determine the recovery and reproducibility of the method under multilaboratory conditions. Since there were no restrictions regarding the type of analytical instrumentation to use for the analyses, laboratories used a combination of equipment that included GC/MS, GC/MS/MS, and LC/MS/MS instruments from 22 different manufacturers, 21 brands of GC and LC columns, 13 different GC temperature programming profiles, 11 LC gradient elution programs, and six different vendor manufactured SPE cartridges. Even though all the analytical performance parameters for all the 653 compounds had been determined in the SLV study, guidance was obtained from an expert review panel of the AOAC Method-Centric Committee on Pesticide Residues to conduct the multilaboratory collaborative study based on 20 selected compounds that can be analyzed by GC/MS and 20 compounds that can be analyzed by LC/MS/MS. Altogether, 560 samples covering the 40 selected pesticides were analyzed in the study. These samples included green tea and oolong tea samples fortified typically at the European Union maximum residue limit for regulatory guidance and compliance, aged tea samples incurred with 20 pesticides, and green tea and oolong tea samples incurred with five pesticides. The analysis of the 560 samples generated a total of 82 459 test results by the 30 participating laboratories. One laboratory failed to meet the proficiency requirements in the precollaborative study. Therefore, its data submitted for the collaborative study were excluded from further analysis and interpretation. The results presented are therefore the 6638 analytical results obtained from the 29 remaining laboratories, which included 1977 results generated by GC/MS, 1704 results by GC/MS/MS, and 2957 results by LC/MS/MS. It was determined after application of the Grubbs and Dixon tests for outliers to the data sets that there were 65 outlier results from the 1977 GC/MS results (3.3%), 65 outlier results from the 1704 GC/MS/MS results (3.8%), and 57 outlier results out of 2957 LC/MS/MS results (1.9%), representing 0.98, 0.98, and 0.86%, respectively, of the 6638 results generated in the study. Analysis with the AOAC statistical software package also confirmed that the method is rugged, and average recovery, average concentration, RSDr, RSDR, and HorRat values all meet recovery and reproducibility criteria for use in multiple laboratories. The Study Director is recommending this method for adoption as an AOAC First Action Official MethodSM.
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Sujana, I. Putu. "The application of biochar to screen printing liquid waste polluted land, its effect in soil, mustard greens to heavy metals (Fe, Cr)." Research Journal of Textile and Apparel 22, no. 3 (September 10, 2018): 224–34. http://dx.doi.org/10.1108/rjta-02-2018-0006.

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Purpose The purpose of this paper is to analyse the screen printing liquid waste polluted soil physical, chemical and biological characteristics, with the unpolluted soil, and to analyse the application of some types of biochar towards the growth of mustard greens plants and the concentration of heavy metals Fe, Cr on the screen printing liquid waste polluted soil. Design/methodology/approach This research was conducted in a green house by using fully randomized design, split plot design pattern, with three replications. The main plot is the type of biochar, and the subplot is the dosage of biochar. The biochar consists of four types (B1 = chicken manure biochar, B2 = coconut shell biochar, B3 = rice hulls biochar and B4 = mahogany woods biochar). The dosage of biochar consists of four levels (D0 = control, D1 = 5 ton/hectare, D2 = 10 ton/hectare and D3 = 15 ton/hectare). The tested variable is being analysed by using analysis of variance (ANOVA). Findings The screen printing liquid waste polluted soil physical, chemical and biological characteristics analysis shows that the soil pH is neutral, a low C organic, a low N total, a high P, CEC and base saturation, while the texture is soft. The analysis results of rice hulls biochar physical, chemical and biological characteristics are quantitatively better in comparison with chicken manure biochar, coconut shell biochar and mahogany biochar. The quantitative application of rice hulls biochar15 ton/hectare dosage can increase the growth of mustard greens, and also, it recovers the soil characteristics by heavy metals total rate of 14.11 ppm Fe and 0.95 ppm Cr from the plant, while 209.05 ppm Fe and 4.12 ppm Cr were found in the soil. Originality/value This is one of few studies the biochar to screen printing liquid waste polluted lands. Currently, numerous kinds of chemical substances have been applied in a form of fertilizer and pesticide into the soil. Other activities like transporting the crop residues, and the contamination of irrigation water that is caused by screen printing liquid waste, have also affected the soil. It becomes degraded where the soil becomes compact and losses its nutrients, and it is containing heavy metals material that is toxic for plants. Biochar is applied into the polluted soil to improve the soil, which is hard to decompose and is long-lasting in the soil. These days, both the raw or ready food products are exposed to the heavy metals with a large and concerning number, especially in big cities which most of the soil is polluted.
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Bjørge, Christine, Marit Låg, Ragna Bogen Hetland, Agnethe Christiansen, Lise Skrettberg, Åshild K. Andreassen, Augustine Arukwe, et al. "Comparison of Organic and Conventional Food and Food Production Part V: Human Health – Pesticide Residues." European Journal of Nutrition & Food Safety, February 26, 2019, 99–101. http://dx.doi.org/10.9734/ejnfs/2019/v9i230045.

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The present report is based on data from the 2010 EFSA Report on pesticide residues in food, the Norwegian monitoring programmes 2007-2012 and data from peer reviewed literature and governmental agencies. It is a challenge to perform quantitative estimates and comparative studies of residue levels due to large variation in the measured levels, and the large number of different pesticides present in the samples. Thus, the focus is on the frequency of observed contaminations in relation to regulatory limits and to present examples to illustrate the variation in residue values and number of detected substances. Pesticide residues in conventional and organic products: Of the 12,168 samples (plant- and animal products) in the 2010 EU-coordinated programme, 1.6% exceeded the respective maximum residue level (MRL) values, and 47.7% had measurable residues above the limit of quantification (LOQ), but below or at the MRL. Of the 1168 samples analysed in Norway in 2012 (from both imported and domestic products), 1.9% exceeded MRL and 53% contained measurable pesticide residues. Direct comparison of these values is however not possible, since they contain different types of food samples, and are analysed for a different number of pesticides. When organic and conventional samples from fruit, vegetables and other plant products in the 2010 EU-coordinated programme were compared, 4.2% of the conventional and 1.0% of the organic samples exceeded the MRL values, while 43.2% of the conventional and 10.8% of the organic samples had measurable residues below or at the MRL value. Most of the pesticide residues detected in organic samples are not permitted for use in organic farming. Of the 624 organic samples analysed in Norway 2007 - 2012, 0.2% (one sample) had residues exceeding MRL, while measurable residues were detected in 1.8% of the samples (11 samples). Conventional products were often found to contain different pesticides while most organic samples were found to contain few or only one type of pesticide. Lack of data on pesticide residue levels of organic samples in the EU-coordinated programme, and few Norwegian samples do not allow for a quantitative comparison of pesticide residue levels in organic and conventional samples. Comparative estimation of pesticide residues faces a number of challenges and uncertainties. However, it seems unquestionable based on available data that organic plant products contain fewer and substantially lower amounts of pesticide residues than conventional products. Health risk associated with pesticide residues: The general level of pesticide residues in both conventional and organic food is low, and well below what is likely to result in adverse health effects. This conclusion is based on the comparison of estimated dietary exposure with toxicological reference values i.e. acceptable daily intake (ADI) for chronic effects, and acute reference dose (ARfD) for acute effects. The finding of pesticide residues that exceeds established regulatory limits in a minority of tested samples is not considered to represent a health risk. When dietary exposure that was estimated in six different food commodities in the 2010 EUcoordinated programme was compared with their relevant reference values, EFSA concluded that for 79 of 18243 conventionally grown fruit and vegetable samples, a short-term acute consumer health risk could not be excluded. The conclusion was based on the exceeding of ARfD. None of these 79 samples were organic. It is important to also consider that the exceeding of the acute reference value only occurred in 0.4% of the samples and that the scenario used for acute intake assessment is conservative, suggesting that the toxicological implications are limited. This is also reflected in the chronic exposure assessment, where none of the samples were found to exceed the toxicological reference value ADI. Dietary exposure assessments on the basis of Norwegian samples of apples, tomatoes, carrots, strawberries and lettuce did not show an exceeding of any toxicological reference value. Combined exposure and cumulative risk assessment of pesticide residues: No generally accepted methodology is at present established for cumulative risk assessment of combined exposure to pesticide residues. Available data suggest however that combined exposure is not likely to result in increased human health risk.
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43

Jiang, Mengmeng, Haicheng Gao, Xinxin Liu, Yu Wang, Jiaqi Lan, Yuanxiang Li, Ketong Zhu, Pingsheng Gong, and Shaowu Lv. "Detection of pesticide residues in vegetables sold in Changchun City，China." Journal of Food Protection, October 27, 2020. http://dx.doi.org/10.4315/jfp-20-236.

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In this essay we investigate mainly 18 pesticide residues with different chemical structures in fresh vegetables, including organochlorine pesticides, organophosphorus pesticides, carbamate pesticides and pyrethroid pesticides. At the same time, it is estimated that the potential health risks for residents. A total of 313 samples were collected from 12 kinds of vegetables from Changchun, the capital of Jilin Province,China. 18 pesticide residues in 313 samples were analyzed by Gas chromatography and mass spectrometry (GC-MS) . Testing linearity was favorable in the range of 0.01 - 1.00μg/mL, R 2 ≥0.99, and the recovery rate of pesticides was 62% - 110%, the relative standard deviation < 5%, the detection limit of the pesticide is 0.0001 - 0.0167 mg / kg, the limit of quantification is 0.0002 - 0.0556 mg / kg. Overall, the detection rate of pesticides was 28.43%, and the detection rate and over-standard rate of celery were the highest, while the pesticide detection rate of potatoes was the lowest, and the pesticide exceeding rate of cucumber was the lowest. Three pesticides tested were not detected in the 18 pesticides including heptachlor, chlorpyrifos and permethrin. Among the 15 pesticides detected, the maximum risk factor of 7 pesticides is greater than 1 such as carbofuran, omethoate, phorate, dicofol, dimethoate, chlorpyrifos and dichlorvos, which may cause potential harm to human health. In contrast others will be safe. It could not have significant perniciousness for people from the perspective of single pollution level,, but it is not ignored there are multiple pesticide residue compound pollution to endanger persons' health.
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44

Dwaidy, Jana, Dina Cheaib, Adla Jammoul, and Nada El Darra. "Assessment of phenolic content, pesticide residue and biological activities of organic lemon and cucumber in Lebanese market." Nutrition & Food Science ahead-of-print, ahead-of-print (June 10, 2021). http://dx.doi.org/10.1108/nfs-01-2021-0013.

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Purpose This study aims to evaluate the safety and quality of organic food product versus conventional ones in the Lebanese market. Design/methodology/approach Selected organic and conventional Lemon and cucumber were assessed for the presence of pesticides residues using LC-MS/MS and GC/MS/MS, also compared at the level of total polyphenols content, flavonoids, tannins and tested for their antiradical and antibacterial activities. Findings The findings indicate that organic lemons were contaminated by four types of pesticide residues (33.33%), while one pesticide residue (22.22%) was detected in conventional one, which were all below the European Union Maximum Residue Limits. For cucumber, six pesticide residues (66.66%) were detected in organic samples, while in conventional, eight pesticide residues (55.55%) were detected. However, absolutely four samples (44.44%) in each of conventional and organic cucumber samples surpass the maximum residue levels. Both lemon and cucumber, regardless of the farming systems, possess potent antioxidant activity with no significant difference, except for lemon, where total polyphenol was highly significant in conventional. Additionally, this study showed that lemon of conventional origin was slightly more effective in inhibiting the growth of gram-positive and gram-negative bacterial strains compared to organic samples, while both cucumber types did not exert any antibacterial effect. Originality/value This is the first paper to assess the polyphenols, pesticide residue and biological activities of organic lemon and cucumber in Lebanese market as well as comparing conventional to organic.
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45

"Tentative guidelines for testing the bioavailability and toxicological potential of grain‐bound pesticide residues." Journal of Environmental Science and Health, Part B 27, no. 4 (August 1992): 427–31. http://dx.doi.org/10.1080/03601239209372793.

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46

Eyring, Philipp Rudolf Michael Peter, Susan Strange Herrmann, and Mette Erecius Poulsen. "Multiresidue analysis of 184 pesticides in high-fat fish feed using a new generic extraction method coupled with gas and liquid chromatography-tandem mass spectrometry." Applied Biological Chemistry 64, no. 1 (April 26, 2021). http://dx.doi.org/10.1186/s13765-021-00610-9.

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AbstractAnimal feed is typically plant-based and can contain pesticide residues. Methods for testing food and feed samples, such as the Quick Easy Cheap Effective Rugged Safe (QuEChERS) method or the Swedish Ethyl Acetate (SweEt) method, successfully extract many pesticide residues. However, nonpolar pesticides, such as organochlorine pesticides, show poor recovery when extracted from lipid-rich samples. The previously developed water-acetonitrile-heptane-solid-phase-extraction (WAHSPE) method shows better recoveries for the nonpolar pesticides but requires two injections per sample and per instrument. Here, we present a modified version of the WAHSPE method for pesticides in fish feed using one injection per sample and per instrument. Of the 184 pesticides tested, 179 met the European Union Legislation’s validation criteria at a spike level of 50 μg/kg, showing recoveries between 70 and 120% and a relative standard deviation (RSD) below 20%. Organochlorine pesticides accounted for 14 of the tested compounds.
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47

Elobeid, Tahra, Vijay Ganji, Sara Al-Saeedi, Alaa Abdelmonem Mohamed, Hana Mohamed Dahir, Hassan Hassan, Layal Karam, and Grace Attieh. "Pesticide residues in foods and water in Qatar and their impact on food exposure risk assessment." British Food Journal ahead-of-print, ahead-of-print (May 21, 2021). http://dx.doi.org/10.1108/bfj-01-2021-0040.

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PurposeThe purposes of this study were to analyze fruits, vegetables, water and soil for organochlorine pesticide (OCP) residues and to assess the food exposure of these pesticides in Qatar.Design/methodology/approachPesticides were quantified in dates, leafy vegetables, fruiting vegetables, water and soil samples using a gas chromatography-electron capture detector and gas chromatography-mass spectrometry. These pesticides were α-benzene hexachloride (BHC), ß-BHC, heptachlor, aldrin, g-chlordane, endosulfan I, α-chlordane, dieldrin, endrin and methoxychlor. Additionally, food exposure risk assessment was performed by estimating daily intakes of OCP.FindingsMost analyzed samples contained at least one OCP residue. Endosulfan was the only pesticide that was not detected. The concentrations of OCP in samples were below the maximum residue level (MRL) except endosulfan. Among all the samples analyzed, ˜18% of those exceeded the MRL with respect to the concentrations of methoxychlor and heptachlor. Only intake of methoxychlor (0.018 mg/day) exceeded the MRL (0.01 mg/day). Dates and fruiting vegetables were likely to pose a higher risk than leafy vegetables because they contained heptachlor, endrin and methoxychlor. Leafy vegetables might pose a greater risk than dates and fruiting vegetables because of the presence of β-BHC and dieldrin.Originality/valueEight out of ten OCPs that were measured were found to be below the MRL. These pesticides should be eliminated from the food supply based on the Qatar National Implementation Plan of the Stockholm Convention in 2010. Based on the intake risk assessment, overall, the intake of OCP may not pose a major risk to human health as the concentrations of OCP were below MRL, except methoxychlor. Water and soil are the potential sources of contamination of OCP in foods that were tested in Qatar. To limit the health risks associated with OCPs, there is a need for close monitoring of food and agricultural practices and the types of pesticides imported into Qatar.
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48

Daniel, V. N., M. Charles, and P. M. Dass. "Risk Assessment of Organochlorine Residues in Agricultural Crops Cultivated [2020] on/around Abandoned Tin Mine Areas in Jos South LGA, Plateau State, Nigeria." International Research Journal of Pure and Applied Chemistry, July 1, 2021, 24–35. http://dx.doi.org/10.9734/irjpac/2021/v22i530407.

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Aims: To investigate the levels and the associated risks of 18 organochlorine residues in water, soil, sediment, and five vegetables cultivated on abandoned mine areas. Study Design: Water, sediment, soil (at 0 -10cm, 11 – 20cn, 21 – 30cn) and vegetables samples were collected from the abandoned tin mine agricultural areas. These subsamples were separately combined and mixed so that a portion taken of the composite was representative of each subsample. The representative fractions were then treated for analysis Place and Duration of Study: Samples were collected between February and May 2020 from the cultivated abandoned mine areas in Du, Jos - South Local Government Area, Plateau State, Nigeria, Methodology Liquid–liquid extractions methods were used for the extraction of pesticide residues from water, sediment, soil and vegetables. The organochlorine residues were determined by GC/MS. Results: The physico- chemical properties data obtained for the soils/sediment from abandoned mine sites in Jos South were very heterogeneous, hence, various behaviors of pesticide residues in different soil/sediment matrices. There were no significant differences (P= 0.05) in mean minerals among the various samples. The pesticides residues detected in water were b-endosulfan, p,p-DDD and methoxychlor. The residues recorded in water were above the WHO’s MRL and Federal Food, Drug and Cosmetic Act (FFDCA,) for drinking water. Residues were also detected in sediment and soils samples. The 11 – 20cm subsoil accumulated the highest levels of the pesticide analyzed. The order of the accumulation of the OCP were; y-BHC>DDD>endrin>endrin ketone>a-endosulfan>b-endosulfan and of the sample type was water<surface soil<21-30cm subsoil<sediment<11-20cm subsoil. The results also showed the presence of OCPs in potato, tomato, cabbage, green beans, and green peppers. y-BHC in potato, tomato and green pepper, endrin in tomato, endrin ketone in potato, tomato and green beans and d-BHC in cabbage had EDI higher levels than ADI and so their HQ greater than 1. The health risks indices (HRI) less than 1 in all other OCP residues were obtained for adults and children that would consume the vegetables except for y-BHC and endrin ketone in potato and tomato, d-BHC in cabbage, d- BHC in green pepper and green beans where the HRI is above 1 that poses health risk. There is however no significant difference (P=0.05) among vegetable types. Positive correlation values ( 0.72, 0.83, 0.71, and 0.56) were observed between endrin and lindane, endrin and heptachlor, endrin and DDT respectively. Conclusion: The consumption of vegetables that contained y-BHC, d-BHC, endrin and endrin ketone whose EDI and HQ were greater than 1 could pose non-carcinogenic health risks. Adults are likely to have less health risk from consuming these vegetables. The effective monitoring of pesticide residues in food items is required. There is also need to sensitize and educate the general public especially the end-users (farmers) on management practices of pesticides.
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Chow, Willis, Daniel Leung, and Jian Wang. "A Complementary, Quantitative and Confirmatory Method to UHPLC/ESI Q-Orbitrap Screening based on UPHLC/ESI-MS/MS for Analysis of 416 Pesticides in Fruits and Vegetables." Journal of AOAC INTERNATIONAL, September 27, 2021. http://dx.doi.org/10.1093/jaoacint/qsab116.

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Abstract Background Triple quadrupole (MS/MS) and high-resolution mass spectrometer (HRMS), coupled with ultra-high performance liquid chromatography (UHPLC) or gas chromatography (GC), are technologies used to analyse pesticide residues in fruits and vegetables. LC-MS/MS has been the gold standard for analysis of pesticides, offering reliable performance and sensitivity, while LC-HRMS is expanding in applications to serve as another benchmark. Method development and testing scope expansion are constantly required with new generation mass spectrometers. Objective This paper discusses the development and validation of a quantitative and confirmatory method that can analyse over 400 pesticide residues using state-of-the-art UHPLC/ESI-MS/MS system. Method Homogenized fruit and vegetable samples were fortified with pesticides and were extracted using a modified QuEChERS method. Samples were injected onto a UHPLC/ESI-MS/MS system, and data were acquired in multiple reaction monitoring mode. The method was validated using a nested experimental design, and was able to quantify and confirm 416 pesticide in fruits and vegetables. It was also complimentary to the UHPLC/ESI Q-Orbitrap quantitative and screening methods previously developed in the authors’ laboratory. Results The method demonstrated good performance. In all matrices, 92% of pesticides yielded recoveries between 81–110%, more than 95% of pesticides yielded intermediate precision ≤ 20%, and about 65% of pesticides yielded measurement uncertainties ≤ 20%, and 96% of pesticides yielded measurement uncertainties ≤ 50%. Highlights This method was developed using the same mobile phases, analytical columns, and extraction procedure, as UHPLC/ESI Q-Orbitrap methods. Extracts can be run on either system, streamlining monitoring programs and offering high sample throughput.
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50

Edwin, O. Clarke, O. Adeboyejo Akintade, P. Ndimele Emeka, and M. Olarinmoye Oluwatosin. "Assessment of Persistent Organochlorine Pesticide Residues in Commercially Important Fin and Shell Fishes of River Majidun, Lagos, Nigeria." Current Journal of Applied Science and Technology, March 4, 2021, 142–53. http://dx.doi.org/10.9734/cjast/2021/v40i131244.

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Aim: The pesticide pollution of aquatic ecosystems has developed serious environmental anxiety, provoking a necessity for continuous evaluation of harmful constituents. Study Design: A quantitative cum descriptive experimental design was used to evaluate the occurrence and concentration of Persistent Organochlorine Pesticides (POPs) in water, sediment, fish (Tilapia zilli and Chrysichthys nigrodigitatus) and shell fishes (Macrobrachium vollenhovenii, Littorina littorea and Callinectes pallidus) of River Majidun, Lagos, Nigeria. Place and Duration of Study: Nigerian Institute of Oceanography and Marine Research (NIOMR) between June and December, 2019. Methodology: Sediment samples were collected by the Rigosha grab sampler and fish samples were purchased from commercial fishermen. Sample preparation was done according to the Environmental Protection Agency (US EPA) 3570 method. POPs were evaluated using Hewlett Packard 5890 series II gas chromatography with electron capture detector. Results: Twenty-one organochlorine residues were identified including p’p’DDT, Lindane (γ-HCH), Dieldrin, Heptachlor, Aldrin, Chlordane, Endrin aldehyde, Endrin ketone, Methoxichlor and Endosulphan. Concentrations in water ranged between 0.03 µg l-1 (Endrin ketone) and 1.97 µg l-1 (Methoxychlor). In sediment, it is between 4.55 µg kg-1 (β-HCH) and 128.25 µg kg-1 (Methoxychlor). In Macrobrachium vollenhovenii, Methoxychlor was 123.83 µg kg-1 and Lindane ((γ)- HCH) was highest here (39.35 µg kg-1). Callinectes pallidus had a high concentration of Endrin ketone (133.13 µg kg-1). The Tilapia zilli highest concentration was 110.35 µg kg-1 (endrin ketone) and it had the highest pp’DDT which was 41.40 µg kg-1. Conclusion: Evidently, there was sequestration of POPs from water into sediment and bioaccumulation in the organisms, due to exposure. The level of POPs in all samples were below the limits of 200 µg kg-1 fresh weight in fish and sea food set by Codex Alimentarius Commission by FAO/WHO. The attendant environmental/human menace cum inherent danger of the raised levels of POPs, calls for continuous monitoring of River Majidun.
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