Determination of Emerging Contaminants in Cereals by Gas Chromatography-Tandem Mass Spectrometry.

Cereals are staple foods for human consumption in both developed and developing countries. In order to improve agricultural outputs, resources like reclaimed water for irrigation and biosolids and manure as fertilizers are frequently used, although they may increase the input of contaminants that can potentially be absorbed by crops and enter the food chain. Emerging contaminants (human and veterinary pharmaceuticals, personal care products, surfactants, plasticizers, and industrial additives, among others) are continuously introduced in the environment from a variety sources and these contaminants may enter the food chain through plant uptake.

Assessing the benefits of composting poultry manure in reducing antimicrobial residues, pathogenic bacteria, and antimicrobial resistance genes: a field-scale study.

The poultry industry in the European Union produces 13 million tons of manure annually, which represents a major health and environmental challenge. Composting is an environmental-friendly technique for the management of manure, but there are few studies about antibiotic residues and antimicrobial resistances at a field scale. The goal of this study was to determine if the composting of poultry manure at a field scale would result in the reduction of antibiotic residues, pathogenic bacteria, and antibiotic resistance genes (ARGs) in the final fertilizer product.

Analysis of Multiclass Antibiotics in Lettuce by Liquid Chromatography-Tandem Mass Spectrometry to Monitor Their Plant Uptake.

The main entry routes of antibiotics in the environment are the application of organic wastes to improve soil quality and the irrigation with recycled water. Once in the environment, antibiotics can be introduced in the food chain through their uptake by crops. This paper describes the development of an analytical method based on ultrasound-assisted extraction for the determination of seven antibiotics in lettuce.

Rapid determination of antibiotic residues in cereals by liquid chromatography triple mass spectrometry.

Antibiotics may be present in agricultural soils through the application of organic amendments as fertilizers or by irrigation of fields with recycled water. As a result of these agricultural practices, antibiotics in soil can lead to their uptake by plants, entering in this way the food chain. Studies on the levels of antibiotics in cereal samples are scarce in the available literature.

Molecularly imprinted polymer-hollow fiber microextraction of hydrophilic fluoroquinolone antibiotics in environmental waters and urine samples.

In the present work, the preparation of a new selective molecularly imprinted polymer (MIP) for the family of fluoroquinolones (FQs) in the pores of polypropylene hollow fibers (HFs) is proposed. The resulting MIP-HFs, which combine solid-phase microextraction (SPME) and molecular imprinting technologies, were used to develop a selective microextraction methodology (MIP-HFM) to determine selected FQs danofloxacin, norfloxacin, enrofloxacin and ciprofloxacin in real samples of environmental and biological interest. Measurements during the optimization of the MIP-HFM and its application to the analyses of real samples were performed by HPLC-UV and HPLC-MS/MS.

Persistence and availability of veterinary antibiotics in soil and soil-manure systems.

The availability and persistence of various antibiotics in soil and soil amended with composted poultry manure were investigated through laboratory incubation assays. Six veterinary antibiotics (one fluoroquinolone, two tetracyclines, two sulfonamides and one lincosamide) and one active metabolite (ciprofloxacin) were studied. The incubation assays were conducted at a controlled temperature of 25 °C with different water regimes, such as constant moisture content (80% of water holding capacity) and drying-rewetting cycles.

Analysis of emerging organic contaminants in poultry manure by gas chromatography-tandem mass spectrometry.

A multiresidue method was developed for the determination of 19 emerging organic contaminants (pharmaceutical drugs, personal care products, and bisphenol A) in poultry manure. Lyophilized samples of manure were extracted by ultrasound-assisted matrix solid-phase dispersion and the extracts were analyzed by gas chromatography with tandem mass spectrometry after derivatization. Analysis of spiked poultry manure samples, at levels ranging from 25 to 150 ng/g, gave satisfactory recovery results for all the compounds, with values from 67 to 106%.

Analysis of macrolide antibiotics in water by magnetic solid-phase extraction and liquid chromatography-tandem mass spectrometry.

Macrolides are one of the most commonly used families of antibiotics employed in human and veterinary treatment. These compounds are considered emerging contaminants with potential ecological and human health risks that could be present in surface water. This paper describes the development and application of a simple and efficient extraction procedure for the determination of tilmicosin; erythromycin, tylosin and erythromycin-HO from water samples.

Rapid multiresidue determination of bisphenol analogues in soil with on-line derivatization.

Bisphenol analogues are compounds extensively used which have been potentially linked to adverse health effects. Nevertheless, few studies reported the analysis of compounds, other than bisphenol A, in environmental solid samples and none in soil samples. In this study, a rapid and sensitive analytical method is presented for the simultaneous determination of 13 bisphenols in soil samples.

Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry.

A rapid extraction procedure is presented for the determination of five endocrine-disrupting compounds, estrone, ethinylestradiol, bisphenol A, triclosan, and 2-ethylhexylsalicylate, in water samples. The analysis involves a two-step extraction procedure that combines dispersive liquid-liquid microextraction (DLLME) with dispersive micro-solid phase extraction (D-μ-SPE), using magnetic nanoparticles, followed by in situ derivatization in the injection port of a gas chromatograph coupled to triple quadrupole mass spectrometry. The use of uncoated or oleate-coated FeO nanoparticles as sorbent in the extraction process was evaluated and compared.

Application of matrix solid-phase dispersion followed by GC-MS/MS to the analysis of emerging contaminants in vegetables.

A multiresidue method for the determination of 17 emerging contaminants in vegetables was developed based on ultrasound-assisted matrix solid-phase dispersion (MSPD). The analysis was performed using isotope dilution gas chromatography tandem mass spectrometry. In the development of the MSPD procedure, different parameters such as sonication and the type of sorbent or extraction solvent were assayed.

Simultaneous determination of multiclass emerging contaminants in aquatic plants by ultrasound-assisted matrix solid-phase dispersion and GC-MS.

A multiresidue method was developed for the simultaneous determination of 31 emerging contaminants (pharmaceutical compounds, hormones, personal care products, biocides, and flame retardants) in aquatic plants. Analytes were extracted by ultrasound-assisted matrix solid-phase dispersion (UA-MSPD) and determined by gas chromatography-mass spectrometry after sylilation, The method was validated for different aquatic plants (Typha angustifolia, Arundo donax, and Lemna minor) and a semiaquatic cultivated plant (Oryza sativa) with good recoveries at concentrations of 100 and 25 ng g wet weight, ranging from 70 to 120 %, and low method detection limits (0.3 to 2.

Uptake of azoles by lamb's lettuce (Valerianella locusta L.) grown in hydroponic conditions.

An uptake and translocation study of azole compounds was performed in lamb's lettuce (Valerianella locusta L.) grown in nutrient solution fortified with different azoles. Three azoles, (clotrimazole, fluconazole and propiconazole), which have different physico-chemical properties and are ubiquitous in the aquatic environment, were the compounds selected.

Application of magnetic iron oxide nanoparticles for the analysis of PCBs in water and soil leachates by gas chromatography-tandem mass spectrometry.

Two magnetic solid-phase extraction methods (mSPE) were developed and compared for the extraction and preconcentration of polychlorinated biphenyls (PCBs) from water and soil leachates. Analyses were carried out by gas chromatography coupled to triple quadrupole mass spectrometry. The mSPE extraction parameters were optimised using Fe3O4 nanoparticles coated with palmitate or oleate.

Multiresidue analysis of insecticides and other selected environmental contaminants in poultry manure by gas chromatography/mass spectrometry.

An analytical method was developed for the simultaneous determination in poultry manure of 41 organic contaminants belonging to different chemical classes: pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and polybrominated diphenyl ethers. Poultry manure was extracted with a modified QuEChERS method, and the extracts were analyzed by isotope dilution GC/MS. Recovery of these contaminants from samples spiked at levels ranging from 25 to 100 ng/g was satisfactory for all the compounds.

Rapid determination of natural and synthetic hormones in biosolids and poultry manure by isotope dilution GC-MS/MS.

The release of hormones into the environment due to land application of biosolids and manure is a cause of concern for their potential impacts. This paper presents the development of a rapid and sensitive method, based on extraction, for the analysis of 13 hormones in biosolids and poultry manure. A simultaneous derivatization of hydroxyl and ketone groups was carried out for the determination of hormones by GC–MS/MS.

Determination of selected pharmaceutical compounds in biosolids by supported liquid extraction and gas chromatography-tandem mass spectrometry.

In this work, an analytical method was developed for the determination of pharmaceutical drugs in biosolids. Samples were extracted with an acidic mixture of water and acetone (1:2, v/v) and supported liquid extraction was used for the clean-up of extracts, eluting with ethyl acetate:methanol (90:10, v/v). The compounds were determined by gas chromatography-tandem mass spectrometry using matrix-match calibration after silylation to form their t-butyldimethylsilyl derivatives.

Occurrence and analysis of selected pharmaceutical compounds in soil from Spanish agricultural fields.

This work describes the analysis of 15 pharmaceutical compounds, belonging to different therapeutic classes (anti-inflammatory/analgesics, lipid regulators, antiepileptics, β-blockers and antidepressants) and with diverse physical-chemical properties, in Spanish soils with different farmland uses. The studied compounds were extracted from soil by ultrasound-assisted extraction (UAE) and determined, after derivatization, by gas chromatography with mass spectrometric detection (GC-MS). The limits of detection (LODs) ranged from 0.

Fast ultrasound-assisted extraction combined with LC-MS/MS of perfluorinated compounds in manure.

A fast analytical method for the determination of perfluorinated compounds in poultry manure by LC-MS/MS was developed. The extraction was carried out by ultrasound-assisted extraction of 1 g of sample, during 2 × 15 min using low volume (5.5 mL) of a mixture of methanol and acetonitrile.

A rapid procedure for the determination of C60 and C70 fullerenes in soil and sediments by ultrasound-assisted extraction and HPLC-UV.

In this work, a rapid and sensitive method, based on ultrasound-assisted extraction of samples with a small volume of toluene, has been developed for the quantification of C60 and C70 fullerenes in soil and sediments. Good extraction efficiencies were obtained at all of the fortification levels studied (200, 100, 20 and 2 ng/g), which ranged from 72 to 104%. An important effect of the extraction temperature was observed on C60 recoveries, and an acceptable decrease in the recovery rates was observed in aged samples.

Analysis of natural-occurring and synthetic sexual hormones in sludge-amended soils by matrix solid-phase dispersion and isotope dilution gas chromatography-tandem mass spectrometry.

A sensitive analytical method is presented for the simultaneous determination of four synthetic estrogens and six steroid hormones in sludge-amended soil. The method employs matrix solid-phase dispersion (MSPD) followed by isotope dilution gas chromatography-tandem mass spectrometry injecting a large volume sample (10μL) after trimethylsilyl derivatization, using the solvent vent mode. It affords good resolution, high sensitivity and reproducibility and freedom from interferences even from complex matrices as soil amended with sewage sludge.

Review of sample preparation techniques for the analysis of pesticide residues in soil.

This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination.

Gas chromatography-triple-quadrupole mass spectrometry for analysis of selected polyhalogenated pollutants in plants. Comparison of extraction methods.

Different extraction methods, followed by gas chromatography coupled to triple quadrupole mass spectrometry, were evaluated for simultaneous extraction of seven polychlorinated biphenyls (PCBs) and six polybrominated diphenyl ethers (PBDEs) from common weeds. Pressurized liquid extraction (PLE) with in-cell clean-up, ultrasound-assisted extraction (UAE) with in-column clean-up, and UAE with dispersive solid-phase extraction (dSPE) clean-up were evaluated and compared. In-cell clean-up with 4 g Florisil and 0.

Determination of selected organic contaminants in soil by pressurized liquid extraction and gas chromatography tandem mass spectrometry with in situ derivatization.

The determination of organic contaminants in soil is a real challenge due to the large number of these compounds with quite different physico-chemical properties. In the present work, an analytical method was developed for the simultaneous determination in soil of 40 organic contaminants belonging to different chemical classes: polycyclic aromatic hydrocarbons, polychlorinated biphenyls, polybrominated diphenyl ethers, UV filters, parabens, bisphenols and triclosan. Soil was extracted by pressurized liquid extraction and the extracts, without the need of a clean-up step, were analyzed by gas chromatography-tandem mass spectrometry after in situ derivatization in the gas chromatographic system.

Occurrence and analysis of parabens in municipal sewage sludge from wastewater treatment plants in Madrid (Spain).

A rapid method for determination of seven parabens and two chlorinated by-products in sewage sludge was developed based on matrix solid-phase dispersion and gas chromatography-tandem mass spectrometry. The analytical procedure showed good recoveries that ranged from 80 to 125%, with relative standard deviations lower than 12% and low detection limits, ranging from 0.1 to 2.