Applications of Experimental Design to the Optimization of Microextraction Sample Preparation Parameters for the Analysis of Pesticide Residues in Fruits and Vegetables

2015 ◽  
Vol 98 (5) ◽  
pp. 1171-1185 ◽  
Author(s):  
Lukman Bola Abdulra'uf ◽  
Ala Yahya Sirhan ◽  
Guan Huat Tan
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Fruits And Vegetables ◽  
Current Trend ◽  
Cost Effective ◽  
Multivariate Statistical ◽  
Analytical Methodology ◽  
Microextraction Techniques ◽  
Doehlert Matrix ◽  
Preparation Techniques

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.

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

2014 ◽  
Vol 97 (4) ◽  
pp. 1007-1011 ◽  
Author(s):  
Lukman Bola Abdulra'uf ◽  
Guan Huat Tan
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Internal Standard ◽  
Calibration Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Design Matrix ◽  
Analytical Methodology ◽  
Cocoa Powder

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%.

Review of Sample Preparation Techniques for the Analysis of Pesticide Residues in Soil

2012 ◽  
Vol 95 (5) ◽  
pp. 1258-1271 ◽  
Author(s):  
José L Tadeo ◽  
Rosa Ana Pérez ◽  
Beatriz Albero ◽  
Ana I García-Valcárcel ◽  
Consuelo Sánchez-Brunete
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Method Development ◽  
Solid Phase ◽  
Soil Extracts ◽  
Assisted Extraction ◽  
Ultrasonic Assisted ◽  
Cleanup Procedure ◽  
Ultrasonic Assisted Extraction ◽  
Preparation Techniques

Abstract This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination. The optimization of sample preparation is a very important part of the method development that can reduce the analysis time, the amount of solvent, and the size of samples. This review considers all aspects of sample preparation, including extraction and cleanup. Classical extraction techniques, such as shaking, Soxhlet, and ultrasonic-assisted extraction, and modern techniques like pressurized liquid extraction, microwave-assisted extraction, solid-phase microextraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are reviewed. The different cleanup strategies applied for the purification of soil extracts are also discussed. In addition, the application of these techniques to environmental studies is considered.

Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables

2010 ◽  
Vol 1217 (16) ◽  
pp. 2548-2560 ◽  
Author(s):  
Steven J. Lehotay ◽  
Kyung Ae Son ◽  
Hyeyoung Kwon ◽  
Urairat Koesukwiwat ◽  
Wusheng Fu ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Fruits And Vegetables ◽  
Preparation Methods ◽  
Sample Preparation Methods

scholarly journals Pesticide Residues in Canned Foods, Fruits, and Vegetables: The Application of Supercritical Fluid Extraction and Chromatographic Techniques in the Analysis

2003 ◽  
Vol 3 ◽  
pp. 1314-1326 ◽  
Author(s):  
Mohamed H. EL-Saeid
Keyword(s):  
Supercritical Fluid Extraction ◽  
Supercritical Fluid ◽  
Pesticide Residues ◽  
Fruits And Vegetables ◽  
Cost Effective ◽  
Food Samples ◽  
Fluid Extraction ◽  
Consumer Safety ◽  
Canned Foods ◽  
Multiple Pesticide Residues

Multiple pesticide residues have been observed in some samples of canned foods, frozen vegetables, and fruit jam, which put the health of the consumers at risk of adverse effects. It is quite apparent that such a state of affairs calls for the need of more accurate, cost-effective, and rapid analytical techniques capable of detecting the minimum concentrations of the multiple pesticide residues. The aims of this paper were first, to determine the effectiveness of the use of Supercritical Fluid Extraction (SFE) and Supercritical Fluid Chromatography (SFC) techniques in the analysis of the levels of pesticide residues in canned foods, vegetables, and fruits; and second, to contribute to the promotion of consumer safety by excluding pesticide residue contamination from markets. Fifteen different types of imported canned and frozen fruits and vegetables samples obtained from the Houston local food markets were investigated. The major types of pesticides tested were pyrethroids, herbicides, fungicides, and carbamates.By using these techniques, the overall data showed 60.82% of the food samples had no detection of any pesticide residues under this investigation. On the other hand, 39.15% different food samples were contaminated by four different pyrethroid residues ± RSD% ranging from 0.03 ± 0.005 to 0.05 ± 0.03 ppm, of which most of the pyrethroid residues were detected in frozen vegetables and strawberry jam. Herbicide residues in test samples ranged from 0.03 ± 0.005 to 0.8 ± 0.01 ppm. Five different fungicides, ranging from 0.05 ± 0.02 to 0.8 ±0.1 ppm, were found in five different frozen vegetable samples. Carbamate residues were not detected in 60% of investigated food samples. It was concluded that SFE and SFC techniques were accurate, reliable, less time consuming, and cost effective in the analysis of imported canned foods, fruits, and vegetables and are recommended for the monitoring of pesticide contaminations.

Recent achievements and applications of solid – phase microextraction in pesticide residues analysis in food

2015 ◽  
Vol 8 (2) ◽  
pp. 178-190
Author(s):  
Mária Andraščíková ◽  
Svetlana Hrouzková
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Solid Phase Microextraction ◽  
Method Development ◽  
Solid Phase ◽  
Current Trend ◽  
Preparation Methods ◽  
Pesticides Residues ◽  
Fiber Coating ◽  
Food Matrices

Abstract The current trend in sample preparation methods is devoted to minimizing or eliminating the volume of extractive solvent. In this review, the focus on solid phase microextraction (SPME) as a solvent free sample preparation method for the isolation of pesticides residues in different food matrices is given. To achieve satisfactory extraction efficiency, selection of the fiber coating is an important step in the method development. Here, recent trends in new supporting materials and new fiber coatings development are discussed. Finally, applicability of SPME for the pesticide residues analysis in various food matrices using mainly chromatographic methods is also reviewed.

scholarly journals Design of experiment in the development of spme method for the determination of pesticide residues in fruits and vegetables

2015 ◽  
Vol 2 (1) ◽  
Author(s):  
Lukman Bola Abdulra’uf ◽  
Guan Huat Tan
Keyword(s):  
Fruits And Vegetables ◽  
Method Development ◽  
Solid Phase ◽  
Current Trend ◽  
Gas Chromatography Mass Spectrometry ◽  
Highly Sensitive ◽  
Sensitivity And Selectivity ◽  
Microextraction Techniques ◽  
Experimental Runs

AbstractThe various microextraction techniques have been developed in order to reduce sample preparation time, improve sensitivity and selectivity as well as to corroborate the recent advances in the development of highly sensitive and efficient analytical instrumentation. The current trend is aimed at the simplification and miniaturization of extraction steps, which has led to the combination of multi-step extraction and analytical analysis into single uninterrupted step. The method development involves the screening and subsequent optimization of both gas chromatography-mass spectrometry (GC-MS) and solid phase microextraction (SPME) parameters using multivariate experimental design, which has been shown to be efficient and effective with little experimental runs. The use of microextraction has been very effective in the analysis of contaminants in food, water and the environments to ensure they are safe and does not pose any health risk to human.

scholarly journals Food processing as a means for pesticide residue dissipation

2016 ◽  
Vol 31 (3-4) ◽  
pp. 89-105 ◽  
Author(s):  
Tijana Djordjevic ◽  
Rada Djurovic-Pejcev
Keyword(s):  
Food Processing ◽  
Pesticide Residues ◽  
Fruits And Vegetables ◽  
Health Hazard ◽  
Cumulative Effect ◽  
Cost Effective ◽  
Penetration Ability ◽  
Effect Of Food ◽  
Thermal Degradation Product ◽  
Processing Techniques

Pesticides are one of the major inputs used for increasing agricultural productivity of crops. However, their inadequate application may produce large quantities of residues in the environment and, once the environment is contaminated with pesticides, they may easily enter into the human food chain through plants, creating a potentially serious health hazard. Nowadays, consumers are becoming more aware of the importance of safe and high quality food products. Thus it is pertinent to explore simple, cost-effective strategies for decontaminating food from pesticides. Various food processing techniques, at industrial and/or domestical level, have been found to significantly reduce the contents of pesticide residues in most food materials. The extent of reduction varies with the nature of pesticides, type of commodity and processing steps. Pesticides, especially those with limited movement and penetration ability, can be removed with reasonable efficiency by washing, and the effectiveness of washing depends on pesticide solubility in water or in different chemical solvents. Peeling of fruit and vegetable skin can dislodge pesticide residues to varying degrees, depending on constitution of a commodity, chemical nature of the pesticide and environmental conditions. Different heat treatments (drying, pasteurization, sterilization, blanching, steaming, boiling, cooking, frying or roasting) during various food preparation and preservation processes can cause losses of pesticide residues through evaporation, co-distillation and/or thermal degradation. Product manufactures, from the simplest grain milling, through oil extraction and processing, juicing/pureeing or canning of fruits and vegetables, to complex bakery and dairy production, malting and brewing, wine making and various fermentation processes, play a role in the reduction of pesticide contents, whereby each operation involved during processing usually adds to a cumulative effect of reduction of pesticides present in the material. There is diversified information available in literature on the effect of food processing on pesticide residues which has been compiled in this article.

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