Countless environmental pollutants and xenobiotics, are widespread and linked to hazardous effects, including breast cancer. Due to their lipophilic properties, these accumulate in fat tissue, such as breast adipose tissue. However, little is still known about their combined effects and distribution within the breast microenvironment. Alterations in fatty acid metabolism can be a biomarker for cancer progression and a potential bioindicator of pollutant exposure. In this study, the fatty acid profile and levels of organochlorine and organophosphate pesticides (OCPs and OPPs), polychlorinated biphenyls (PCBs), brominated flame retardants (BFRs), organophosphate esters (OPEs), polycyclic aromatic hydrocarbons (PAHs) and synthetic musks (SMs) were measured in 48 breast adipose tissue samples from breast cancer and healthy patients (controls). Twelve xenobiotics were detected at high frequency rates, and the distribution profile of these pollutants differed between cohorts. In total, 163 correlations were identified between specific fatty acids and breast cancer patients' data, with distinct correlation patterns between cohorts. Fatty acids show the potential to be biomarkers of the presence of lipophilic xenobiotics in the breast microenvironment; however, more studies are needed. This preliminary study is the first to analyze OPPs, OPEs, and PAHs in breast adipose tissue and report associations between xenobiotics and specific fatty acids.

The use of a polypyrrole (PPy) is described as an efficient extraction phase for disposable pipette extraction (DPX), in a fast and ruggedized analytical method for simultaneous determination of 18 organic micro-pollutants in water using gas chromatography-mass spectrometry (GC-MS). The DPX-blank pipettes were filled with PPy, a material produced through the chemical polymerization of PPy using iron(III) chloride hexahydrate. The optimized conditions were 5 extraction cycles with 600 µL of sample, adjusted to pH 9, and desorption with 150 µL of ethyl acetate using 7 cycles with the same aliquot. The calibration curves resulted in determination coefficient (R2) higher than 0.9963, the limit of detection (LOD) ranged from 0.4 to 1.5 µg L−1, and the limit of quantification (LOQ) were from 1.4 to 5.0 µg L−1. Excellent results were obtained for repeatability (2.3 to 15%, for 5 µg L−1) and intermediate precision, varying the day of analyses (3.9 to 15.5%) and the pipette tip (3.4 to 22.4%). The analyte recovery ranged from 75.4 to 115.0% for river water, and from 74.9 to 116.2% for tap water, in three different levels of concentration. The DPX-GC-MS method with PPy was successfully applied to determine the 18 analytes in river and tap water from the cities of Joinville and Florianópolis, Santa Catarina, Brazil.

Brazilian citrus essential oils (mandarin, orange, lemon, bergamot and tangerine) were analyzed for the determination of pesticides residues of organochlorine (aldrin, chlordane, dieldrin and dicofol) and organophosphorus (methyl chlorpyrifos, dimethoate, methidathion and methyl parathion) . A comparative study between gas chromatography-mass spectrometry in selective ion monitoring mode (GC-MS-SIM) and gas chromatography-electron capture detector (GC-ECD) was performed using solid phase extraction (SPE) with Florisil® cartridge for the pre-concentration of pesticides. The average recovery of pesticides was from 71 to 83% as determined by GC-MS-SIM analysis and 99 to 104% by GC-ECD. The limit of quantification was from 0.93 to 3.93 mg L-1 in GC-MS-SIM and 0.09 to 0.12 mg L-1 in GC-ECD. Fifteen samples of commercial Brazilian citrus essential oils were analyzed and six samples showed contamination with values above the maximum residue limit (MRL) allowed by the Codex Alimentarius.

In this work, the chemically modified filter paper with polyaniline/polypyrrole (PANI/PPY), denoted as PANI/PPY/cellulose nanocomposite, was prepared and used as the solid phase extraction (SPE) sorbent for preconcentration and extraction of some organochlorine pesticides (OCPs) in natural water samples. The proposed sorbent was also characterized with scanning electron microscopy (SEM) and exhibited that globular polymers could incorporate into the cellulose fibers of the paper sheet. Several experimental parameters related to the preconcentration of OCPs on the coated filter paper were also examined. The experimental results showed that the PANI/PPY coated filter paper could extract OCPs with relatively high enrichment factors. The evaluation also exhibited a dynamic range of 5-250 µg L-1 for OCPs with proper correlation coefficient (R²). The limit of detections of heptachlor, aldrin, dieldrin, endrin and 4-dichlorodiphenyltrichloroethane (4-DDT) were found to be 0.39, 0.28, 0.47, 0.51 and 0.31 µg L-1, respectively. The proposed method was also applied for analysis of OCPs in seawater sample and the recoveries of analytes were in the range of 77.4 to 102.7 %.

A method based on headspace - solid phase microextraction coupled with gas chromatography - mass spectrometry was validated for the quantitative determination of 18 organochlorine pesticides in water. For the extraction conditioning some parameters as the best type of coating fiber, time and temperature of extraction, pH and ionic strength were evaluated. The method HS-SPME/GC-MS/MS showed linear coefficient above 0.9948. The repeatability of the measurements were lower than 7.6%. Relative recoveries were between 88 and 110%. Limits of detection from 0.5 x 10-3 to 1.0 mg L-1 were obtained. A total of 31 samples were analyzed and 16 presented from 1 to 5 pesticides.

A method using Gas Chromatography coupled to Mass Spectrometry (GC-MS) for the determination of hexachlorobenzene, lindane, heptachlor, heptachlor epoxide, aldrin, dieldrin, endrin, 4,4'-DDT and 4,4'-DDE in leaves of Mikania laevigata, Maytenus ilicifolia and Cordia verbenacea was developed. Extraction of the pesticides was carried out by solid-liquid extraction (SLE), followed by clean-up in solid phase mixed cartridge (Florisil and silica-gel). Quantification was performed using GC-MS in the selected ion monitoring mode. Mean recovery rates of 70 to 124% were obtained. The inter-assay precision of a sample fortified with 200 ng g-1 of each pesticide was in the range of 1.0 to 7.3%. The quantitation limits ranged from 3.0 to 30 ng g-1 and were below the Maximum Residue Limit (MRL) for all the pesticides under study. The method was employed to analyze samples of Mikania laevigata, Maytenus ilicifolia and Cordia verbenacea from an experimental field in Paulínia, SP, Brazil. The samples presented contamination with dieldrin above the MRL established by the European Pharmacopoeia (50 ng g-1).

This paper proposes a method based on matrix solid phase dispersion (MSPD) to determine the presence of organochlorine (OC) and organophosphorus (OP) pesticide residues in species of Passiflora L. (passion fruit) leaves by gas chromatography, using an electron capture detector (HRGC-ECD). A comparison with conventional methods, mainly the European Pharmacopoeia method (EP), showed MSPD to be efficient, fast, simple and easy to perform. To date, there are no official methods or limits that take into account Brazil's "real life" conditions in the analysis of pesticides in medicinal plants and phytomedicines, and the MSPD method described herein has proved to be a feasible one for the analysis of Passiflora L-based phytomedicines.

Abstract In this study, we investigated the differences between the gilthead bream fishes that live in cages and feed by fish feed (CF), had escaped from the cages and started to live in their natural medium (EF), and live in their natural medium and do not feed by fish feed (NF). We would like to demonstrate the micro pollutants and heavy metal residues in CF, EF and NF and reveal out the diversity in living in three different ambient conditions. We analyzed Mn, Cr, Zn, Sn, Ag, Hg, Cd, Cu, Ni and Pb residues and p-p’-DDE, α-BHC, endosulfan-sulfate, endrin, heptachlor, heptachlor epoxide, methoxychlor, p-p’-DDD, p-p’-DDT, β-BHC, aldrin, cypermethrin, dieldrin ve endosulfan pesticides in three types of gilthead bream (CF, EF and NF) and also researched the heavy metal residues in the marine sample that provided from Guvercinlik Cove in three different time intervals by gas chromatography-mass spectroscopy (GC-MS) and Inductively Coupled Plasma-Mass Spectrometer (ICP-MS). Physical and chemical parameters of sea water samples were studied to reveal out the effect of fish feed between the regions. Heavy metal and organochlorine pesticides residues of gilthead bream muscle tissues from CF are remarkable higher than other regions when we evaluate the all results. The results show an indication of the significant health risks associated with the consumption of these contaminated fish in the cages. The morphology of gilthead bream fish liver tissue samples were studied by using scanning electron microscopy (SEM).

The development and validation of a simultaneous liquid-liquid extraction method for organochlorine pesticides and trihalomethanes in surface and drinking water by HRGC-ECD is described. The method presents acceptable recovery, with detection ranging from 2.7 to 49.0 ng L-1 for organochlorine pesticides and from 18.0 to 860.0 ng L-1 for trihalomethanes. The extraction method also presents excellent linearity for all the analytes, with excellent repeatability. Extraction is simple, fast, and low cost, uses small amounts of solvent and aqueous sample, and is suitable for routine analyses.

A rapid and efficient analytical method is presented for the quantitative analysis of 10 organochlorine pesticides in corn meal. The extraction and clean up steps are combined into one step by transferring the sample to a chromatographic column prepacked with alumina and silica gel. The pesticides are eluted with n-hexane-dichloromethane 9:1 (v/v) and the extracts analized by gas-liquid chromatography with electron capture detection, the average recoveries were between 78% and 98% and the detection limits were between 1 and 5 ng/g.