Targeted and non-targeted analysis of pesticides and aflatoxins in baby foods by liquid chromatography coupled to quadrupole Orbitrap mass spectrometry

Prata, Rafaela; López‐Ruiz, Rosalía; Petrarca, Mateus Henrique; Godoy, Helena Teixeira; Frenich, Antonia Garrido

doi:10.1016/j.foodcont.2022.109072

Cited by 24 publications

(9 citation statements)

References 29 publications

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“…22 A generic gradient previously developed was employed to separate the maximum number of compounds as possible. 21 Mobile phases were slightly different: methanol and water containing 0.1% formic acid. Myclobutanil was eluted at 7.95 min (Figure S2).…”

Section: Resultsmentioning

confidence: 99%

“…Chromatographic and spectrometric parameters are summarized in Table . To obtain as much information as possible, a generic separation method previously optimized was used . Thus, water containing 0.1% formic acid (Eluent A) and methanol (Eluent B) were used as mobile phases, the flow rate was set at 0.3 mL/min, and the elution gradient was as follows: gradient started with 95% of A and was kept constant for 1 min.…”

Section: Methodsmentioning

confidence: 99%

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Looking beyond the Active Substance: Comprehensive Dissipation Study of Myclobutanil-Based Plant Protection Products in Tomatoes and Grapes Using Chromatographic Techniques Coupled to High-Resolution Mass Spectrometry

Marín-Sáez

López‐Ruiz

Romero-González

et al. 2022

J. Agric. Food Chem.

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A comprehensive evaluation of the dissipation of a myclobutanil plant protection product was performed in tomato and grape samples. Different temperature conditions (3 and 22 °C) were evaluated. A biphasic kinetic model provided a suitable adjustment (R 2 > 0.95), with persistence (residual level, RL 50 ) lower than 24 days in all cases. Solid−liquid extraction and ultra-highperformance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap-HRMS) were used for metabolites' elucidation, identifying six myclobutanil metabolites, four out of them described for the first time and one of them confirmed using 1 H, 13 C, ( 1 H-1 H)-COSY, ( 1 H-13 C)-HMQC, and ( 1 H-13 C)-HMBC nuclear magnetic resonance (NMR). Their degradation curves were also evaluated, increasing their concentrations when the myclobutanil concentration decreases. Additionally, coformulants present in the commercial formulation were monitored employing headspace solid-phase microextraction method (HS-SPME)-gas chromatography coupled to HRMS (GC-Q-Orbitrap-HRMS). Seven coformulants were quantified in tomato samples. Their dissipation curves were studied, and it was observed that they were almost degraded 12 days after application.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Looking beyond the Active Substance: Comprehensive Dissipation Study of Myclobutanil-Based Plant Protection Products in Tomatoes and Grapes Using Chromatographic Techniques Coupled to High-Resolution Mass Spectrometry

Marín-Sáez

López‐Ruiz

Romero-González

et al. 2022

J. Agric. Food Chem.

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“…Mobile phases were composed of methanol (eluent A) and water 0.1% formic acid (eluent B) at a flow rate of 0.3 mL/min. The chromatographic gradient employed was previously developed . Briefly, from 95% of B (1 min), the percentage was decreased to 0% in 3 min and kept constant for 6 min.…”

Section: Methodsmentioning

confidence: 99%

“…The chromatographic gradient employed was previously developed. 30 Briefly, from 95% of B (1 min), the percentage was decreased to 0% in 3 min and kept constant for 6 min. Then, it was increased to 95% (0.5 min) and kept constant for 3.5 min.…”

Section: Instruments and Apparatusmentioning

confidence: 99%

Comprehensive Dissipation of Azadirachtin in Grapes and Tomatoes: The Effect of Bacillus thuringiensis and Tentative Identification of Unknown Metabolites

Marín-Sáez

López‐Ruiz

Romero-González

2023

J. Agric. Food Chem.

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Neem oil is a biopesticide normally applied together with Bacillus thuringiensis (Bt). However, neither its dissipation nor the influence of Bt has been previously evaluated. In this study, dissipation of neem oil was investigated when it was applied alone or together with Bt at 3 and 22 °C. A methodology involving solid–liquid extraction and liquid chromatography-high-resolution mass spectrometry was developed for that purpose. The method was validated obtaining recoveries from 87 to 103%, with relative standard deviations lower than 19% and limits of quantification from 5 to 10 μg/kg. Azadirachtin A (AzA) dissipation was fit to a single first order, being faster when neem oil was applied together with Bt and at 22 °C (RL50 = 12–21 days) than alone and at 3 °C (RL50 = 14–25 days). Eight related compounds were found in real samples with similar dissipation curves compared to AzA, and five unknown metabolites were identified in degraded samples, with increasing concentrations during parent compound degradation.

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“…Currently, CYP residues in various samples are mainly detected by instrument methods, including high-performance liquid chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) [ 11 , 12 ]. These well-established chromatographic methods demonstrate excellent detection limits and reliable accuracy for effective monitoring of CYP residues.…”

Section: Introductionmentioning

confidence: 99%

Development of Ic-ELISA and Colloidal Gold Lateral Flow Immunoassay for the Determination of Cypermethrin in Agricultural Samples

Huang

Zhang

et al. 2022

Biosensors

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Cypermethrin (CYP) is an insecticide in the pyrethroid family and is used widely in agriculture and for public health purposes. However, CYP has been shown to have negative impacts on reproduction, immunity and nerves in mammals. In this study, a monoclonal antibody (mAb) against CYP was prepared and used to establish an indirect competitive immunosorbent assay (ic-ELISA) and colloidal gold lateral flow immunoassay (LFIA) for the quantitative and qualitative determination of CYP residues in agricultural products. The half inhibition concentration of the ic-ELISA was 2.49 ng/mL, and the cut-off value and visual limit of detection of the LFIA were 0.6 and 0.3 μg/mL, respectively. The recovery rates of the ic-ELISA ranged from 78.8% to 87.6% in tomato, cabbage and romaine lettuce. The qualitative results of LFIA and quantitative results of ic-ELISA and HPLC were in good agreement in blind samples. Overall, the established ic-ELISA and LFIA proved to be accurate and rapid methods for the determination of CYP in agricultural products.

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Targeted and non-targeted analysis of pesticides and aflatoxins in baby foods by liquid chromatography coupled to quadrupole Orbitrap mass spectrometry

Cited by 24 publications

References 29 publications

Looking beyond the Active Substance: Comprehensive Dissipation Study of Myclobutanil-Based Plant Protection Products in Tomatoes and Grapes Using Chromatographic Techniques Coupled to High-Resolution Mass Spectrometry

Looking beyond the Active Substance: Comprehensive Dissipation Study of Myclobutanil-Based Plant Protection Products in Tomatoes and Grapes Using Chromatographic Techniques Coupled to High-Resolution Mass Spectrometry

Comprehensive Dissipation of Azadirachtin in Grapes and Tomatoes: The Effect of Bacillus thuringiensis and Tentative Identification of Unknown Metabolites

Development of Ic-ELISA and Colloidal Gold Lateral Flow Immunoassay for the Determination of Cypermethrin in Agricultural Samples

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