Method validation and comparison of acetonitrile and acetone extraction for the analysis of 169 pesticides in soya grain by liquid chromatography–tandem mass spectrometry

Pizzutti, Ionara Regina; Kok, Albert; Hiemstra, Maurice; Wickert, Cristine; Prestes, Osmar D.

doi:10.1016/j.chroma.2009.03.064

Cited by 102 publications

(45 citation statements)

References 21 publications

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“…A fast, easy, and efficient method with acceptable performance for the analysis of 169 pesticides in soya grain using LC-QqQ-MS in positive (155 pesticides) and negative (14) ESI mode in a single chromatographic run has been reported (Pizzutti et al, 2007(Pizzutti et al, , 2009). In two other cases, multi-residue methods have been developed for the simultaneous determination of less than fifty pesticides in bovine whole milk using LC-QqQ-MS acquiring the MRM transitions, both in positive and negative ESI mode (Bogialli et al, 2006;Dagnac et al, 2009).…”

Section: Ms Analysis Of Pesticidesmentioning

confidence: 98%

Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices

Botitsi¹,

Garbis

Economou

et al. 2010

Mass Spectrometry Reviews

153

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Analysis of pesticides and their metabolites in food and water matrices continues to be an active research area closely related to food safety and environmental issues. This review discusses the most widely applied mass spectrometric (MS) approaches to pesticide residues analysis over the last few years. The main techniques for sample preparation remain solvent extraction and solid-phase extraction. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) approach is being increasingly used for the development of multi-class pesticide residues methods in various sample matrices. MS detectors-triple quadrupole (QqQ), ion-trap (IT), quadrupole linear ion trap (QqLIT), time-of-flight (TOF), and quadrupole time-of-flight (QqTOF)-have been established as powerful analytical tools sharing a primary role in the detection/quantification and/or identification/confirmation of pesticides and their metabolites. Recent developments in analytical instrumentation have enabled coupling of ultra-performance liquid chromatography (UPLC) and fast gas chromatography (GC) with MS detectors, and faster analysis for a greater number of pesticides. The newly developed "ambient-ionization" MS techniques (e.g., desorption electrospray ionization, DESI, and direct analysis in real time, DART) hyphenated with high-resolution MS platforms without liquid chromatography separation, and sometimes with minimum pre-treatment, have shown potential for pesticide residue screening. The recently introduced Orbitrap mass spectrometers can provide high resolving power and mass accuracy, to tackle complex analytical problems involved in pesticide residue analysis.

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Section: Ms Analysis Of Pesticidesmentioning

confidence: 98%

Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices

Botitsi¹,

Garbis

Economou

et al. 2010

Mass Spectrometry Reviews

153

View full text Add to dashboard Cite

show abstract

“…Different studies demonstrated that some of them, such as QuEChERS procedure, based on acetonitrile extraction and dispersive solid phase extraction, are appropriate for liquid chromatography-mass spectrometry (LC-MS) analysis but problematic for gas chromatography-mass spectrometry (GC-MS). These facts were demonstrated by various studies [5,10,11]. Other methods, based on single extraction like ethyl acetate (EtOAc) method, are appropriate for GC-MS analysis of most matrices but generate problems in the case of pigmented samples due the tendency of EtOAc to extract many pigments and volatiles substances from matrices [5,11].…”

Section: Introductionmentioning

confidence: 99%

Multiresidue Analysis of Pesticides and Metabolites from Fruits and Vegetables by Gas Chromatography—Time-of-Flight Mass Spectrometry

Meghesan-Breja¹,

Cimpoiu²,

Hosu³

2015

Acta Chromatographica

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Summary. This work describes the comparison of five sample extraction methods for the determination of pesticide residues in grapes and vegetables by using gas chromatography-time-of-flight mass spectrometry (GC-TOF-MS). These methods were based on original methods QuEChERS, mini-Luke, ethyl acetate, and DIN EN 15637, and some of these were slightly modified to increase the number of identified and quantified pesticides, to improve their quantification limits, and to be fast and less expensive in terms of material cost. The acceptable performance parameters combined with the properties of easy and quick handling and cost-effectiveness have made mini-Luke modified extraction method as the most favorable in the pesticide residues analysis from grapes and tomatoes by GC-TOF-MS. The efficiency of the chosen extraction method was also verified for lettuce; for this matrix, a cleanup step with graphitized black carbon (GBC) was added. Analysis of extracts was carried out by GC-TOF-MS within 29.2 min run time. The GC method was validated for grapes and tomatoes in terms of linearity, accuracy, limit of detection (LOD), and limit of quantification (LOQ). Good linearity with correlation coefficients (r 2 ) higher than 0.98 was obtained. For most analytes from both matrices, recoveries were in the range of 71-120% and LOQ values in the range of 0.01-0.05 mg kg −1 . The GC-TOF-MS and modified mini-Luke extraction methods were successfully tested on real vegetable and fruit samples belonging to the same commodities group as those from validated methods according to European Guide DG SANCO 12571/2013 (tomatoes, pepper, cucumber, potatoes, carrots, eggplants, onion, lettuce and grapes) and in proficiency EU tests.

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“…15,16 The matrix effect is the effect observed by the increase or decrease in detector response for a particular analyte present in the matrix extract compared to the detector response for the analyte in organic solvent. 17 In this study, the matrix effect was evaluated in two different ways. The first way was by comparison of peak areas obtained from analytical solutions prepared in organic solvent and from those in blank matrix extract at each individual concentration, according to equation 2.…”

Section: Matrix Effect Evaluationmentioning

confidence: 99%

Pesticide Residues Method Validation by UPLC-MS/MS for Accreditation Purposes

Pizzutti¹,

Dias²,

Kok³

et al. 2016

Journal of the Brazilian Chemical Society

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The development and validation of an analytical method for the determination of 51 pesticides in tomato using UPLC-MS/MS (ultra performance liquid chromatography coupled to tandem mass spectrometry) was performed in order to fulfill the requirements of the NBR ISO/IEC 17025:2005. The goal of the validation was to evaluate all required parameters, such as linearity of analytical curves, instrument and method limits of detection and quantification, matrix effect and accuracy (trueness and precision). Stock solutions of the pesticides were prepared in organic solvent by two different analysts independently, in order to validate this preparation by comparing the detector response areas of injections (n = 7). Pesticides were extracted from tomatoes applying the Dutch mini-Luke method with 30 mL of each solvent as acetone, petroleum ether as well as dichloromethane. A small aliquot of the organic solvent extract was evaporated and reconstituted in methanol with 0.1% of acetic acid (v/v) for UPLC-MS/MS analysis. The recovery experiments were done by spiking blank samples at 10, 20 and 50 µg kg -1 , performed by two analysts, seven replicates for each concentration level plus the blank sample. From the 51 studied compounds, 46 showed recoveries within the acceptable range of 70-120% for all evaluated concentrations. For 82% of pesticides, the validated method limit of quantification was the lowest concentration studied (10 µg kg

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Method validation and comparison of acetonitrile and acetone extraction for the analysis of 169 pesticides in soya grain by liquid chromatography–tandem mass spectrometry

Cited by 102 publications

References 21 publications

Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices

Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices

Multiresidue Analysis of Pesticides and Metabolites from Fruits and Vegetables by Gas Chromatography—Time-of-Flight Mass Spectrometry

Pesticide Residues Method Validation by UPLC-MS/MS for Accreditation Purposes

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