Validation of a multi-residue method and estimation of measurement uncertainty of pesticides in drinking water using gas chromatography–mass spectrometry and liquid chromatography–tandem mass spectrometry

Schwanz, Thiago Guilherme; Carpilovsky, Cristiane Köhler; Weis, Grazielle Castagna Cezimbra; Costabeber, Ijoni Hilda

doi:10.1016/j.chroma.2018.11.058

Cited by 30 publications

(13 citation statements)

References 22 publications

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“…Four different other methods were compared with the present methodregarding the standardization of GC-MS. The present method took 50 min run time in comparison to 70.33 min [16], 60.17 min [24], 60 min [25], 55 min [26]. The less run time ofthepresent method in comparison to others was established.…”

Section: Standardization Of Extractionand Cleaning Up Stepmentioning

confidence: 67%

Validation of a modified QuEChERS method to determine multiclass multipesticide residues in apple, banana and guava using GC–MS and LC–MS/MS and its application in real sample analysis

et al. 2020

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A modified QuEChERS method was developed for the determination of 64 pesticides in apple, guava andbanana using GC-MS and LC-MS/MS. Out of sixty-four pesticides, 39 (32 insecticides + 7 herbicides) were analysed by GC-MS and others were analysed in LC-MS/MS. The efficiency of methanol, ethyl-acetate and acetonitrile as extracting solvents were checked. Among these, acetonitrile gave the highest recovery. d-SPE clean-up was done for apple and guava using PSA, whereas PSA + GCB was used for banana to remove heteropolysaccharides and carotenoids. The method was validated as per SANTE/11813/2017 guidelines. The LOD was in the range of 0.002-0.04 mg kg −1 and LOQ was 0.005-0.11 mg kg −1. Average recovery ranged from 80 to 120% with RSD ≤ 20% and RPD % of precision ≤ 20%. The expanded uncertainty was ≤ 20%. The validated method was applied to check the real samples of apple, guava and banana collected from markets of four different districts of West Bengal, India.

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Section: Standardization Of Extractionand Cleaning Up Stepmentioning

confidence: 67%

Validation of a modified QuEChERS method to determine multiclass multipesticide residues in apple, banana and guava using GC–MS and LC–MS/MS and its application in real sample analysis

et al. 2020

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“…ME is acceptable when it is in range of 80% to 120%. Any value of ME that is outside that range denotes that the matrix effect occurs in the MS measurement [46]. Due to the fact that there is no vegetable-based matrix-certified reference materials for multiclass pesticides commercially available at the moment, the assessment of the matrix effect and recovery of the sample preparation were performed by spiking experiments in this study as the proposal from B.K.…”

Section: Resultsmentioning

confidence: 99%

Multiresidue Pesticides Analysis of Vegetables in Vietnam by Ultrahigh-Performance Liquid Chromatography in Combination with High-Resolution Mass Spectrometry (UPLC-Orbitrap MS)

Vu-Duc

Quang

Le-Minh

et al. 2019

Journal of Analytical Methods in Chemistry

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An ultrahigh-performance liquid chromatography in combination with high-resolution mass spectrometry Thermo Q-Extractive Focus Orbitrap MS has been introduced for analysis of multiclass pesticides in vegetable samples collected in Hanoi, Vietnam. Multiclass pesticides were separated on the Thermo Hypersil Gold PFP column utilizing a gradient of the mobile phase consisting of 5 mM ammonium formate, 0.1% formic acid in deionized water, and methanol. The target analytes were detected in the full-scan mode on Thermo Scientific Q-Exactive Focus Orbitrap MS for quantitation at the optimum operating conditions. These conditions included, but not limit to, the resolution of 70000 at the full width at half maximum in both positive and negative mode, mass range from 80 to 1000 m/z, and optimized parameters for the heated electrospray ionization source. The identification of the analytes in real samples was based on retention times, mass to charge ratios, mass accuracies, and MS/MS spectra at the confirmation mode with the inclusion list of target analytes. The mass accuracies of target analytes were from −4.14 ppm (dinotefuran) to 1.42 ppm (cinosulfuron) in the neat solvent and from −3.91 ppm (spinosad D) to 1.29 ppm (cinosulfuron) in the matrix-matched solution. Target analytes in the vegetable-based matrix were extracted by the QuEChERS method. Some critical parameters of the analytical method such as linearity, repeatability, limit of detection, and limit of quantitation have been evaluated and implemented. Excellent LOD and LOQ of the developed method were achieved at the range of 0.04–0.85 and 0.13–2.9 μg·kg−1, respectively. Intraday and interday repeatability of the analytical signal (peak area, n=6) of the developed method were below 3% and 10%, correspondingly. The matrix effect, extraction recovery, and overall recovery were fully investigated by spiking experiments. Experimental results demonstrated that the ionization suppression or enhancement was the main contribution on the overall recoveries of target analytes. Finally, the in-house validated method was applied to pesticides screening in vegetables samples in local villages in Hanoi, Vietnam. The concentrations of all target analytes were below limit of quantitation and lower than US-FDA or EU maximum residue levels.

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“…It also provides to help the analyst make acceptable decisions. [39][40][41] The uncertainty measurements of each compound in water were determined by using the proposed method. The uncertainty sources in the method were specified to calculate the combined standard uncertainty in compliance with the International Organization for Standardization (ISO) 42 and EURACHEM/Citac 29 guidelines.…”

Section: Measurement Of Uncertaintymentioning

confidence: 99%

Applicability of purge and trap gas chromatography‐ mass spectrometry method for sensitive analytical detection of naphthalene and its derivatives in waters

Güzel

Canlı

2020

J Mass Spectrom

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Nowadays, a wide variety of chemicals has emerged because of increasing industrial and human activities. Thus, environmental chemistry laboratories performing analytical measurements need rapid and sensitive methods more than ever to get reliable quantitative data. For this purpose, a purge and trap gas chromatography–mass spectrometry (GC‐MS) method was developed and validated for the rapid, simple, and sensitive determination of the presence of naphthalene and its derivatives in waters. The method validation was based on specificity, calibration curve linearity, limit of detection (LOD) and limit of quantification (LOQ), accuracy (recovery), precision, matrix effects (MEs), and measurement uncertainty. This method showed excellent linearity from 1.00 to 40.00 μg/L except naphthalene (0.50–40.00 μg/L) because the correlation coefficients were higher than 0.997 for all analytes. The LOQ values varied from 0.312 to 0.746 μg/L, and the LOD values changed from 0.094 to 0.224 μg/L with relative standard deviations (RSDs) for all compounds below 10% (3.12–7.46), respectively. Recoveries ranged from 81.9% to 95.6%, and repeatability and reproducibility (in terms of RSD for six measurements) were lower than 10% in all cases. F test was subjected on the related data at 95% confidence level, and no statistically significant difference was observed. There was no critical ME (recovery varied from 80% to 110% in all matrices). In measurement uncertainty, the expanded uncertainties of each analyte were changed in the range of 0.39–0.52 μg/L, and the calibration curve and repeatability had dominant effects on the combined uncertainty. The application to real samples was successfully assessed by the developed method. These results indicate that the developed method is suitable for the determination of naphthalene and its derivatives in waters.

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Validation of a multi-residue method and estimation of measurement uncertainty of pesticides in drinking water using gas chromatography–mass spectrometry and liquid chromatography–tandem mass spectrometry

Cited by 30 publications

References 22 publications

Validation of a modified QuEChERS method to determine multiclass multipesticide residues in apple, banana and guava using GC–MS and LC–MS/MS and its application in real sample analysis

Validation of a modified QuEChERS method to determine multiclass multipesticide residues in apple, banana and guava using GC–MS and LC–MS/MS and its application in real sample analysis

Multiresidue Pesticides Analysis of Vegetables in Vietnam by Ultrahigh-Performance Liquid Chromatography in Combination with High-Resolution Mass Spectrometry (UPLC-Orbitrap MS)

Applicability of purge and trap gas chromatography‐ mass spectrometry method for sensitive analytical detection of naphthalene and its derivatives in waters

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