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This paper presents a new multi-residue method for the quantification of more than 142 anthropogenic compounds of emerging concern (CECs) in various environmental matrices. These CECs are from a wide range of major classes including pharmaceuticals, household, industrial and agricultural. This method utilises ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) for analysis of five matrices (three liquid and two solid) from wastewater treatment processes and the surrounding environment. Relative recoveries were predominantly between 80 and 120%; however, due to the complexity of the matrices used in this work, not all compounds were recovered in all matrices, from 138/142 analytes in surface water to 96/142 analytes in digested solids. Method quantification limits (MQLs) ranged from 0.004 ng L−1 (bisoprolol in surface water) to 3118 ng L−1 (creatinine in wastewater treatment work (WwTW) influent). The overall method accuracy was 107.0%, and precision was 13.4%. To test its performance, the method was applied to the range of environmental matrices at WwTWs in South West England. Overall, this method was found to be suitable for application in catchment-based exposure-driven studies, as, of the total number of analytes quantifiable in each matrix, 61% on average was found to be above their corresponding MQL. The results confirm the need for analysing both the liquid and solid compartments within a WwTW to prevent under-reporting of concentrations. [ABSTRACT FROM AUTHOR]

During the last few decades, increasing interest in biological surfactants led to an intensification of research for the cost-efficient production of biosurfactants compared with traditional petrochemical surface-active components. The quest for alternative production strains also is associated with new demands on biosurfactant analysis. The present paper gives an overview of existing analytical methods, based on the example of rhamnolipids. The methods reviewed range from simple colorimetric testing to sophisticated chromatographic separation coupled with detection systems like mass spectrometry, by means of which detailed structural information is obtained. High-performance liquid chromatography (HPLC) coupled with mass spectrometry currently presents the most precise method for rhamnolipid identification and quantification. Suitable approaches to accelerate rhamnolipid quantification for better control of biosurfactant production are HPLC analysis directly from culture broth by adding an internal standard or Fourier transform infrared attenuated total reflectance spectroscopy measurements of culture broth as a possible quasi-online quantification method in the future. The search for alternative rhamnolipid-producing strains makes a structure analysis and constant adaptation of the existing quantification methods necessary. Therefore, simple colorimetric tests based on whole rhamnolipid content can be useful for strain and medium screening. Furthermore, rhamnolipid purification from a fermentation broth will be considered depending on the following application. [ABSTRACT FROM AUTHOR]

Analytical techniques for the determination of polychorinated dibenzo- p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF) and dioxin-like PCBs (DLPCB) are reviewed. The focus of the review is on recent advances in methodology and analytical procedures. The paper also reviews toxicology, the development of toxic equivalent factors (TEF) and the determination of toxic equivalent quantity (TEQ) values. Sources, occurrence and temporal trends of PCDD/PCDF are summarized to provide examples of levels and concentration ranges for the methods and techniques reviewed. [ABSTRACT FROM AUTHOR]

This review is devoted to the consideration of prospects and directions for the development of methods and approaches to the analysis of high-purity industrial gases and volatile hydrides, chlorides, fluorides, and organoelement compounds with natural and isotopically enriched compositions. The currently known capabilities for the determination of impurities in them using mass spectrometry, IR spectroscopy, gas chromatography, and chromatography–mass spectrometry are analyzed. [ABSTRACT FROM AUTHOR]

This study reports a liquid phase microextraction method based on binary extraction solvents, which were used to preconcentrate chlorbenside and fenobucarb from aqueous samples for determination by gas chromatography mass spectrometry. Parameters including the type, ratio, and volume of binary solvents, disperser solvent type and volume, and vortex period were optimized systematically to achieve high enrichment for the analytes. The optimum conditions obtained were used to validate the method, and the detection limits calculated for chlorbenside (0.71 ng/mL) and fenobucarb (0.33 ng/mL) correlated to enrichment factors of 399- and 912-folds, respectively. The optimum method was applied to lake water and wastewater samples in spike recovery experiments, and the results obtained (96–104%) verified the method as accurate and applicable to the aqueous sample matrices. Matrix matching calibration method was used to boost the accuracy of quantifying the two analytes in the wastewater sample, which presented interference effects. Assessment of the method's green profile based on penalty points confirmed the method's compliance with green analytical chemistry. [ABSTRACT FROM AUTHOR]

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. In this work, an analytical method was developed for the determination of 19 antibiotics (fluoroquinolones, sulfonamides, tetracyclines, and lincosamides) in four types of cereal grains (wheat, barley, rice, and oat). Ultrasound-assisted matrix solid-phase dispersion was selected as extraction technique with recoveries of target analytes ranging from 73 to 127% for the four cereals analyzed. Limits of quantification obtained ranged from 0.8 to 5.8 ng g−1. Compared with methods described for the analysis of antibiotics in cereals, the developed method uses a lower volume of extraction solvent and very good recoveries were obtained for all compounds. The validated method was applied to the analysis of different types of cereals samples, harvested from agricultural fields or purchased from local supermarkets. The analysis of the five cereal samples grown in fields with 3 years of consecutive organic amendments revealed that none of the nineteen antibiotics selected were found in any sample. Eleven commercial samples of cereals of different types and presentations were analyzed and enrofloxacin was detected in one rice sample; the presence of enrofloxacin in cereals or its incorporation into crops from soil or water not previously reported. [ABSTRACT FROM AUTHOR]

new liquid chromatography-mass spectrometry (LC/MS) method has been developed for the quantitative analysis of plasmalogens in human plasma using a nonendogenous plasmalogen (1- O-1′-( Z)-tricosenyl-2-oleoyl- rac-glycero-3-phosphocholine, PLS 23:0/18:1) as an internal standard. 1- O-1′-( Z)-Tricosenyl glyceryl ether was prepared by reacting lithioalkoxyallyl with 1-iodoeicosane as the key intermediate in the formation of PLS 23:0/18:1. In LC/MS analyses, PLS 23:0/18:1 generated significant fragment ions in positive and negative modes. In positive ion mode, the [M+H] of PLS 23:0/18:1 yielded unique fragments with cleavages at the sn-1 and sn-2 positions of the glycerol backbone. In negative ion mode, the [M+CHCOO] of PLS 23:0/18:1 resulted in characteristic fragmentation at the sn-2 and sn-3 positions. 1- O-1′-( Z)-Hexadecenyl-2-linoleoyl- rac-glycero-3-phosphocholine (PLS 16:0/18:2) and 2-arachidonoyl- O-1′-( Z)-hexadecenyl- rac-glycero-3-phosphocholine (PLS 16:0/20:4) were chemically synthesized as PLS 23:0/18:1. The calibration curves obtained for PLS 16:0/18:2 and PLS 16:0/20:4 were linear throughout the calibration range (0.04-1.60 pmol). The LOD (S/N = 5:1) was 0.008 pmol and the LOQ (S/N = 6:1) was 0.01 pmol for both PLS 16:0/18:2 and PLS 16:0/20:4. Plasma concentrations of PLS 16:0/18:2 and PLS 16:0/20:4 were 4.0 ± 1.3 μM and 3.5 ± 1.2 μM (mean ± SD), respectively, in five healthy volunteers. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

The analysis and presence of clotrimazole, an antifungal agent with log K OW > 4, was thoroughly studied in the aquatic environment. For that reason analytical methods based on gas chromatography–mass spectrometry and liquid chromatography–tandem mass spectrometry were developed and validated to quantify clotrimazole with limits of quantification down to 5 and 1 ng/L, respectively. Both methods were compared in an intercalibration exercise. The complete mass-spectrometric fragmentation pattern could be elucidated with the aid of quadrupole time of flight mass spectrometry. Since clotrimazole tends to adsorb to laboratory glassware, studies on its adsorption behaviour were made to ensure the appropriate handling of water samples, e.g. pH, storage time, pretreatment of sampling vessels or material of the vials used for final extracts. The phenomena of adsorption to suspended matter were investigated while analysing different waste-water samples. Application of the methods in various investigated wastewater and surface water samples demonstrated that clotrimazole could only be detected in the low nanogram per litre range of anthropogenic influenced unfiltered water samples after acidification to pH 2. [ABSTRACT FROM AUTHOR]

An analytical method for the determination of 12 selected estrogens, progestagens and corticosteroids is presented. The optimization of the method, including liquid chromatography separation, extraction on a solid phase, purification on a silica gel cartridge and detection by mass spectrometry, is described. Both the repeatability, with relative standard deviation ranging from 1.4 to 2.7%, and the accuracy, with recoveries ranging from 92.7 to 102.4%, were very satisfactory for ten of the target analytes. The limits of detection were lower than 1 ng/L for progestagens, androgens and corticosteroids, and ranged between 0.9 and 4.3 ng/L for estrogens. The results of the analysis of two sewage treatment plants in the area of Lyon (France) by this method reveal that all the compounds investigated are present in the effluents. The estrogen most frequently detected was estrone, with a median of 26.1 ng/L. The target progestagens were detected with concentrations ranging between 5 and 41 ng/L. Androgens were also present in most of the samples in the range 1–30 ng/L, while the corticosteroids were present only in one plant, with a median of 31.9 ng/L. [ABSTRACT FROM AUTHOR]