Novel Method Development for Extraction and Analysis of Pesticide Residues in Human Serum Samples

In recent years, exposure to pesticides has gained widespread attention due to their adverse health effects. Long-term exposure to pesticides has shown hazardous effects on vital functions of the human nervous and reproductive systems. Therefore, it is crucial to determine the extent of pesticide exposure in humans. Primarily, it is quite challenging to determine trace levels of pesticide residues in biological matrices. Hence, a quick, multi-residue extraction procedure was experimented for pesticide residue analysis in human serum. Herein, the original QuEChERS extraction method was modified for achieving the best possible recoveries. A total of 15 representative pesticides from each class were selected and fortified into the human serum samples. The extraction was performed by employing acidified solution containing acetonitrile and ethyl acetate followed by vortex and centrifugation. The obtained aqueous layer was collected and vapourised to dryness and d-SPE clean-up was conducted utilising PSA. The extracted sample was injected into the GC-MS/MS system under MRM mode. The method development parameters such as linearity, % RSD, accuracy, LOD, LOQ and % ME were assessed. The results obtained for the serum matrix were found to be within the criteria mentioned in European Union SANTE/12682/2019 guidelines for method validation. The developed solitary method is quick, simple and highly efficient for routine pesticide residue analysis. Hence, a wide spectrum of pesticides can be analysed utilising the proposed method for human serum.

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Multi-pesticide residue analysis by high resolution mass spectrometry in complementary matrices: wheat flour, lettuce and apple samples

Analytical Methods ◽

10.1039/c8ay01083h ◽

2018 ◽

Vol 10 (32) ◽

pp. 3958-3967 ◽

Cited By ~ 5

Author(s):

Marilda Chiarello ◽

Sidnei Moura

Keyword(s):

Mass Spectrometry ◽

High Resolution ◽

Human Health ◽

Pesticide Residue ◽

Pesticide Residues ◽

High Resolution Mass Spectrometry ◽

Residue Analysis ◽

Food Contamination ◽

Pesticide Residue Analysis ◽

Resolution Mass

Nowadays, food contamination with pesticide residues is prevalent, which can cause problems to human health.

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Estimation of Measurement Uncertainty in Pesticide Residue Analysis

Journal of AOAC International ◽

10.1093/jaoac/84.5.1569 ◽

2001 ◽

Vol 84 (5) ◽

pp. 1569-1578 ◽

Cited By ~ 29

Author(s):

Lutz Alder ◽

Wolfagang Korth ◽

Alan L Patey ◽

Henk A van der Schee ◽

Siegmar Schoeneweiss

Keyword(s):

Pesticide Residue ◽

Pesticide Residues ◽

Residue Analysis ◽

Pesticide Residue Analysis ◽

Proficiency Tests ◽

Entire Concentration Range ◽

Dependent Relationship ◽

Relative Standard ◽

Residue Concentration ◽

Standard Deviations

Abstract Proficiency test results from 5 countries involving 61 separate interlaboratory proficiency tests for pesticide residues were examined in this study. A total of 24 different matrixes and 869 relative standard deviations of the mean (or median) pesticide residue concentration were statistically evaluated in relation to the Horwitz function. The aim was to determine whether or not the concentration-dependent relationship described by Horwitz would hold for the much narrower range of chemicals and concentrations covered in routine pesticide residue analysis. Although for fatty (animal-derived) matrixes the variability increased as the concentration decreased in line with the Horwitz equation, the between-laboratories relative standard deviations for nonfatty matrixes (fruit, vegetables, and grain) remained at 25% over the entire concentration range of 1 μg/kg to 10 mg/kg for the pesticides studied. Given these findings, the Horwitz equation remains valid for calculating uncertainties involving pesticide residues in fatty matrixes. However, for pesticide residue analyses involving nonfatty matrixes, a constant relative standard deviation of 25% is more appropriate for calculating uncertainties, particularly when a reported result is assessed against a regulatory limit.

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Evaluation of an alternative fluorinated chitosan as a QuEChERS adsorbent for pesticide residue analysis in apple samples

Analytical Methods ◽

10.1039/c9ay00769e ◽

2019 ◽

Vol 11 (27) ◽

pp. 3460-3466 ◽

Cited By ~ 3

Author(s):

Qilin Deng ◽

Liping Sun ◽

Tao Zhu

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Pesticide Residue ◽

Pesticide Residues ◽

High Performance ◽

Residue Analysis ◽

Pesticide Residue Analysis ◽

Quechers Method

In this study, a new and green fluorinated chitosan (trifluoroethyl methacrylate-chitosan (TFEMA-CTS)) was synthesized, and the QuEChERS method was applied for the effective determination of four pesticide residues in apple samples by high performance liquid chromatography.

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Analysis of Pesticide Residues by Polarography

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/48.5.1027 ◽

1965 ◽

Vol 48 (5) ◽

pp. 1027-1037

Author(s):

Raymond J Gajan

Keyword(s):

Pesticide Residue ◽

Pesticide Residues ◽

Residue Analysis ◽

Pesticide Residue Analysis ◽

Stability Studies ◽

Specific Technique

Abstract Polarography is a rapid, sensitive, and relatively specific technique that can be applied to pesticide residue analysis. The technique should also prove a valuable tool in overall pesticide research, such as monitoring new columns, studying kinetics, identifying and determining metabolites, assaying primary pesticide standards, and conducting stability studies.

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Thin-Layer Chromatography for Chlorinated Pesticide Residue Analysis

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/46.5.884 ◽

1963 ◽

Vol 46 (5) ◽

pp. 884-893 ◽

Cited By ~ 1

Author(s):

Martin F Kovacs

Keyword(s):

Liquid Chromatography ◽

Thin Layer ◽

Thin Layer Chromatography ◽

Pesticide Residue ◽

Pesticide Residues ◽

Residue Analysis ◽

Rapid Screening ◽

Gas Liquid Chromatography ◽

Pesticide Residue Analysis ◽

Layer Chromatography

Abstract A rapid sensitive method for the application of thin-layer chromatography to the detection and estimation of chlorinated organic pesticide residues has been developed. Compared to paper chromatography the method is faster, more sensitive, and in most cases more specific. Chlorinated pesticide residues were identified in extracts of various food products at concentrations as low as 1 part per billion; these results were verified by gas-liquid chromatography. Because of its simplicity, speed, and sensitivity, thin-layer chromatography is suitable as a rapid screening method or as a confirmatory method in conjunction with gas-liquid chromatography or other analytical methods for chlorinated pesticide residue analysis.

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Method development for the influence of matrix on selected organochlorine pesticide residue analysis in surface water by GC-MS

Water Pollution XI ◽

10.2495/wp120101 ◽

2012 ◽

Cited By ~ 1

Author(s):

C. Rimayi ◽

F. Mtunzi ◽

C. V. Wyk ◽

D. Odusanya

Keyword(s):

Surface Water ◽

Organochlorine Pesticide ◽

Pesticide Residue ◽

Method Development ◽

Residue Analysis ◽

Organochlorine Pesticide Residue ◽

Pesticide Residue Analysis

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Paper Chromatography in Pesticide Residue Analysis

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/49.3.638 ◽

1966 ◽

Vol 49 (3) ◽

pp. 638-643

Author(s):

D E Coffin

Keyword(s):

Pesticide Residue ◽

Paper Chromatography ◽

Pesticide Residues ◽

Quantitative Estimation ◽

Residue Analysis ◽

Spot Size ◽

Detection Methods ◽

Pesticide Residue Analysis ◽

Advantages And Disadvantages ◽

Chromatographic Techniques

Abstract Some of the paper chromatographic techniques and detection methods used for pesticide residue analysis are reviewed. Procedures utilized for quantitative estimation pesticide residues separated by paper chromatography, such as measurement of spot size, combusion prior to analysis, and elution before chemical analysis, are also discussed. The advantages and disadvantages of paper chromatographic techniques and the problems inherent in the paper chromatographic separation and detection of minute amounts of pesticide residues are outlined. Additional applications and modifications of paper chromatography to extend its usefulness in pesticide residue analysis are suggested.

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A review of sample preparation methods for the pesticide residue analysis in foods

Open Chemistry ◽

10.2478/s11532-012-0034-1 ◽

2012 ◽

Vol 10 (3) ◽

pp. 900-925 ◽

Cited By ~ 32

Author(s):

Lijin Zhang ◽

Shaowen Liu ◽

Xinyi Cui ◽

Canping Pan ◽

Ailin Zhang ◽

...

Keyword(s):

Sample Preparation ◽

Pesticide Residue ◽

Pesticide Residues ◽

Solid Phase ◽

Residue Analysis ◽

Liquid Extraction ◽

Pesticide Residue Analysis ◽

Preparation Methods ◽

Assisted Extraction ◽

Sample Preparation Methods

AbstractThe pesticide residues in foods have received increasing attention as one of the most important food safety issues. Therefore, more strict regulations on the maximum residue limits (MRLs) for pesticides in foods have been established in many countries and health organizations, based on the sensitive and reliable analysis methods of pesticide residues. However, the analysis of pesticide residues is a continuing challenge mainly because of the small quantities of analytes as well as the large amounts of interfering substances which can be co-extracted with them, often leading to experimental errors and damage to the analytical instruments. Thus, extensive sample preparation is often required for the pesticide residue analysis for the effective extraction of the analytes and removal of the interferences. This paper focuses on reviewing the recent development in the sample preparation methods for the pesticide residue analysis in foods since 2006. The methods include: liquid-liquid extraction (LLE), supercritical-fluid extraction (SFE), pressurized-liquid extraction (PLE), microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), gel permeation chromatography (GPC), solid-phase extraction (SPE), molecularly imprinted polymers (MIPs), matrix solid-phase dispersion (MSPD), solid-phase micro-extraction (SPME), QuEChERS, cloud point extraction (CPE) and liquid phase micro-extraction (LPME), etc. Particularly their advantages, disadvantages and future perspectives will be discussed.

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Evaluation of an Automated Gel Permeation Cleanup and Evaluation System for Determining Pesticide Residues in Fatty Samples

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/70.4.724 ◽

1987 ◽

Vol 70 (4) ◽

pp. 724-726

Author(s):

Marvin L Hopper ◽

Kenneth R Griffitt

Keyword(s):

Gas Chromatography ◽

Pesticide Residue ◽

Pesticide Residues ◽

Evaluation System ◽

Residue Analysis ◽

Gel Permeation Chromatography ◽

Pesticide Residue Analysis ◽

Sample Matrix ◽

Fixed Volume ◽

Gel Permeation

Abstract The AutoVap® 600 system, used in conjunction with an automated gel permeation chromatography (GPC) instrument, automatically collects and evaporates the effluent from the GPC column, dissolves the residue in a fixed volume of desired solvent, and quantitatively transfers it to a sealed vial. This system was evaluated and found to automate efficiently the cleanup of butterfat for pesticide residue analysis. Quantitative recoveries were obtained for each of 4 pesticides fortified in butterfat and cleaned up through the system and for 12 pesticide standards in the absence of sample matrix collected through the system. After loading, the system operates unattended and will automatically prepare up to 23 individual fat samples for determination by gas chromatography without additional cleanup.

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