Simultaneous Extraction of Pesticides and Polycyclic Aromatic Hydrocarbons in Brazilian Cachaça Using a Modified QuEChERS Method Followed by Gas Chromatography Coupled to Tandem Mass Spectrometry Quantification

Abstract

A modified QuEChERS method was optimized for simultaneous extraction of 93 pesticides and 6 polycyclic aromatic hydrocarbons (PAHs) in cachaça. The procedure employed 20 mL of sample, 10 mL of dichloromethane, 1 g of NaCl, and 6 g of MgSO4. The methods were validated in accordance with pesticide tolerances set by the National Health Surveillance Agency of Brazil and government guidelines of Brazil and the European Union. The linearity of all curves was adequate, with calculated t r higher than the critical value, at the 95% confidence level. For pesticides, recoveries ranged between 86.7 and 118.2%, relative standard deviation (RSD) ≤ 20%, at least at two concentration levels, and limit of detection (LOD) and limit of quantitation (LOQ) were 2.5 and 10.0 μg L–1, respectively. For PAHs, recoveries ranged between 84.8 and 111.5%, RSD was between 6.2 and 27.3%, LOD and LOQ were 0.25 and 1.0 μg L–1, respectively. The combined standard uncertainty was lower than 50% of the relative expanded uncertainty value at concentration levels of greater relevance in both methods. Analyses of five commercial samples detected the presence of 9 pesticides (10.0–128.0 μg L–1) and 6 PAHs (2.0–4.0 μg L–1), indicating the need for a specific legislation for Brazilian cachaça.

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

“…The LOD and LOQ of all analytes are listed in Table S3 in Supplemental Materials. It should be noted that the developed LOD and LOQ of the method were also comparable with recent publications [41–45].…”

Comprehensive Strategy for Sample Preparation for the Analysis of Food Contaminants and Residues by GC–MS/MS: A Review of Recent Research Trends

“…A new class of PAHs derivatives, known as chlorinated PAHs (Cl-PAHs), have been attracting increasing interest. Emerging Cl-PAHs are also ubiquitous and hazardous pollutants akin to PAHs and other halogenated aromatic compounds, such as polychlorinated dibenzo-p-dioxins, dibenzofurans, and PCBs; the QuEChERS method has been used for sample preparation [120].…”

Analysis of Polycyclic Aromatic Hydrocarbon in Airborne Particulate Matter Samples by Gas Chromatography in Combination with Tandem Mass Spectrometry (GC-MS/MS)

“…Recently, many studies have shown use of gas or liquid chromatography in combination with mass spectrometry such as gas chromatography in combination with electron impact ionization mass spectrometry (GC-EI-MS) [9,10,13], gas chromatography in combination with electron impact ionization tandem mass spectrometry (GC-EI-MS/MS) [14][15][16], liquid chromatography-atmospheric pressure photon ionization tandem mass spectrometry (LC-APPI-MS/MS) [17][18][19], liquid chromatography-fluorescent detector in serial with tandem mass spectrometry (LC-FLD-MS/MS) [20] for analysis of PAHs and their derivative compounds such as nitro-PAHs and hydroxyl-PAHs in both environmental and food sample matrices. Among these methods, GC-EI-MS/MS with excellent selectivity, high sensitivity, and robustness has been a modern and effective method for PAHs analysis in several laboratories.…”

“…Among these methods, GC-EI-MS/MS with excellent selectivity, high sensitivity, and robustness has been a modern and effective method for PAHs analysis in several laboratories. In addition, several sample preparation techniques such as ultrasonic-assisted liquid extraction [2,11,15], traditional Soxhlet extraction, solid phase extraction (SPE) [16,21], pressured solvent extraction (or accelerated solvent extraction, ASE) [10,13], and QuEChERS [9,16,17] have been developed for extraction of PAHs in the real sample matrices prior analysis by gas/liquid chromatography. However, ultrasonic-assisted extraction (UAE) method was considerably used as a green extraction method because of low toxic solvent consumption, high extraction efficiency, and less extraction time, especially for particulate matter or solid samples [22][23][24].…”