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1.
J Chromatogr A ; 1726: 464967, 2024 Jul 05.
Article in English | MEDLINE | ID: mdl-38749275

ABSTRACT

Infant formulas (IF) can contain harmful chemical substances, such as pesticides and mycotoxins, resulting from the contamination of raw materials and inputs used in the production chain, which can cause adverse effects to infants. Therefore, the quick, easy, cheap, effective, rugged, and safe (QuEChERS) methodology prior ultra-high performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPL-QqQ-MS/MS) analysis was applied for the determination of 23 contaminants, in 30 samples of Brazilian IF. The method was validated in terms of limit of detection (0.2 to 0.4 µg/kg), limits of quantification (1 and 10 µg/kg), and recovery (64 % to 122 %); precision values, in terms of relative standard deviation (RSD), were ≤ 20 %. Fenitrothion, chlorpyrifos, and bifenthrin were the pesticides detected in the samples, but the values did not exceed the limit set by the European Union (EU), and ANVISA, and they were detected under their limits of quantification. Additionally, suspect screening and unknown analysis were conducted to tentatively identify 32 substances, including some compounds not covered in this study, such as pesticides, hormones, and veterinary drugs. Carbofuran was identified, confirmed and quantified in 10 % of the samples.


Subject(s)
Food Contamination , Infant Formula , Limit of Detection , Tandem Mass Spectrometry , Tandem Mass Spectrometry/methods , Chromatography, High Pressure Liquid/methods , Brazil , Infant Formula/chemistry , Food Contamination/analysis , Pesticides/analysis , Humans , Pesticide Residues/analysis , Reproducibility of Results , Mycotoxins/analysis , Infant , Pyrethrins/analysis
2.
J Chromatogr A ; 1635: 461757, 2021 Jan 04.
Article in English | MEDLINE | ID: mdl-33302139

ABSTRACT

A simple and effective analytical method to determine six contaminants, including five benzophenones (BP, BP-1, BP-3, BP-8, and BP-12) and bisphenol A (BPA) in infant formulas was developed in this study. For this, a sequential experimental design was used to optimize the extraction and cleanup method using low temperature partition (LTP) combined with dispersive solid phase extraction (dSPE). The effect of primary secondary amine (PSA), sodium chloride (NaCl), graphitized carbon black (GCB), octadecyl (C18), strong anion exchanger (SAX), water, acetonitrile (ACN) and, ultrasound (US) time were evaluated using a sequential design of experiments including a Plackett-Burman, a central composite rotatable design, and the Derringer and Suich's tool. The method was validated, and it showed a limit of quantification varying from 0.06 to 2 mg.kg-1, good precision (< 20% RSD), and recovery (52-106%). The method proposed was applied to twenty-five samples of commercial infant formulas.


Subject(s)
Benzhydryl Compounds/isolation & purification , Benzophenones/isolation & purification , Food Analysis/methods , Infant Formula/chemistry , Phenols/isolation & purification , Solid Phase Extraction , Acetonitriles , Benzhydryl Compounds/analysis , Benzophenones/analysis , Cold Temperature , Food Analysis/instrumentation , Humans , Infant , Limit of Detection , Phenols/analysis
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