Stability of organochlorine pesticides during storage in water and loaded SPE disks containing sediment.

With regard to the Water Framework Directive (WFD) and the required investigation of the whole water sample including suspended particulate matter (SPM), a storage stability study was conducted to determine the suitable storage time and conditions of 21 organochlorine pesticides (OCPs) spiked in water samples and pre-concentrated on solid-phase extraction disks (SPE disks). Furthermore, this work demonstrates the behaviour of three different certified sediment reference materials (CRMs) contaminated with OCPs in water samples as well as loaded on SPE disks under different temperature conditions and storage time periods. Extracts collected on SPE disks were stored for 3, 14 and 30 days at both 4 °C and -18 °C in darkness covered in (a) freezer bags and (b) aluminum foil.

Influence of the drying step within disk-based solid-phase extraction both on the recovery and the limit of quantification of organochlorine pesticides in surface waters including suspended particulate matter.

In this study, 21 organochlorine pesticides (OCPs) were determined based on sample preparation using solid-phase extraction disks (SPE disks) coupled with programmable temperature vaporizer (PTV)-large-volume injection gas-chromatography mass spectrometry (LVI-GC-MS). The work includes a comprehensive testing scheme on the suitability of the method for routine analysis of surface and drinking water including suspended particulate matter (SPM) with regard to requirements derived from the European Water Framework Directive (WFD, Directive 2000/60/EC). SPM is an important reservoir for OCPs, which contributes to the transport of these compounds in the aquatic environment.

Fully automated standard addition method for the quantification of 29 polar pesticide metabolites in different water bodies using LC-MS/MS.

A reliable quantification by LC-ESI-MS/MS as the most suitable analytical method for polar substances in the aquatic environment is usually hampered by matrix effects from co-eluting compounds, which are unavoidably present in environmental samples. The standard addition method (SAM) is the most appropriate method to compensate matrix effects. However, when performed manually, this method is too labour- and time-intensive for routine analysis.

Determination of organic priority pollutants in the low nanogram-per-litre range in water by solid-phase extraction disk combined with large-volume injection/gas chromatography-mass spectrometry.

Polybrominated diphenyl ethers, polychlorinated biphenyls, polycyclic aromatic hydrocarbons and organochlorine pesticides in the low nanogram-per-litre range in water were enriched by solid-phase extraction (SPE) disks and their concentration determined by large-volume injection/gas chromatography-mass spectrometry (LVI/GC-MS). One advantage of using SPE disks in comparison with SPE cartridges is that suspended particulate matter (SPM) does not have to be separated prior to the enrichment step, which saves time and effort. To increase the sensitivity of the method, the SPE disk procedure was combined with LVI/GC-MS, which has not been reported so far for water analysis.

Multi-component trace analysis of organic xenobiotics in surface water containing suspended particular matter by solid phase extraction/gas chromatography-mass spectrometry.

Suspended particulate matter (SPM) often disturbs the analysis of surface water by conventional methods, such as liquid-liquid extraction (LLE) or solid phase extraction (SPE), caused by insufficient extraction or by plugging. Water and SPM are therefore often separately analysed, which is associated with high expenditure of time, work and costs. Hence, SPM is partly ignored, if the fraction of sorptively bound analytes is small compared to the total analyte concentration.

Reduction of matrix effects and improvement of sensitivity during determination of two chloridazon degradation products in aqueous matrices by using UPLC-ESI-MS/MS.

The development and validation of a sensitive and reliable detection method for the determination of two polar degradation products, desphenyl-chloridazon (DPC) and methyl-desphenyl-chloridazon (MDPC) in surface water, ground water and drinking water is presented. The method is based on direct large volume injection ultra-performance liquid chromatography electrospray tandem mass spectrometry. This simple but powerful analytical method for polar substances in the aquatic environment is usually hampered by varying matrix effects, depending on the nature of different water bodies.

Occurrence of residual water within disk-based solid-phase extraction and its effect on GC-MS measurement of organic extracts of environmental samples.

Solid-phase extraction (SPE) is a widespread and powerful sample preparation technique in many analytical areas. Many of the used methods reduce residual water during sample preparation by drying the phase material. Despite the importance of this step, hardly any study deals specifically with the drying process, and if so, only few aspects are mentioned.

Pan-European survey on the occurrence of selected polar organic persistent pollutants in ground water.

This study provides the first pan-European reconnaissance of the occurrence of polar organic persistent pollutants in European ground water. In total, 164 individual ground-water samples from 23 European Countries were collected and analysed (among others) for 59 selected organic compounds, comprising pharmaceuticals, antibiotics, pesticides (and their transformation products), perfluorinated acids (PFAs), benzotriazoles, hormones, alkylphenolics (endocrine disrupters), Caffeine, Diethyltoluamide (DEET), and Triclosan. The most relevant compounds in terms of frequency of detection and maximum concentrations detected were DEET (84%; 454 ng/L), Caffeine (83%; 189 ng/L), PFOA (66%; 39 ng/L), Atrazine (56%; 253 ng/L), Desethylatrazine (55%; 487 ng/L), 1H-Benzotriazole (53%; 1032 ng/L), Methylbenzotriazole (52%; 516 ng/L), Desethylterbutylazine (49%; 266 ng/L), PFOS (48%, 135 ng/L), Simazine (43%; 127 ng/L), Carbamazepine (42%; 390 ng/L), nonylphenoxy acetic acid (NPE(1)C) (42%; 11 microg/L), Bisphenol A (40%; 2.

Determination of the polar pesticide degradation product N,N-dimethylsulfamide in aqueous matrices by UPLC-MS/MS.

This study presents a fast, sensitive, and robust method for the determination of the polar pesticide degradation product N,N-dimethylsulfamide (DMS) in water based on ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). To provide a robust analysis method, the use of an internal standard for both natural waters and model water was examined in order to compensate for matrix effects. The relative standard deviation was found to be +/-15% (n = 10) and the limit of detection was 10 ng/L by direct injection in the UPLC-MS/MS system.

Total concentration analysis of polycylic aromatic hydrocarbons in aqueous samples with high suspended particulate matter content.

The European water framework directive (WFD) requires priority pollutants to be measured in the whole water sample and not only in the dissolved phase. However, it does not give clear definitions on how to achieve this. To overcome this limitation, a new methodology of sample preparation procedure for the analysis of polycyclic aromatic hydrocarbons on the basis of extraction disks is introduced here.

Determination of perfluorooctanoic acid and perfluorooctane sulfonate in Lake Victoria Gulf water.

In this study we present a report of investigation from the screening of perfluorooctanoic acid and perfluorooctane sulfonate in Lake Victoria Gulf and in its source rivers. The first determined levels of perfluorinated alkylated substances in Lake Victoria ecosystem are presented. Variability in the concentrations of perfluorooctanoic acid or perfluorooctane sulfonate in river waters (range perfluorooctanoic acid 400-96,400 and perfluorooctane sulfonate <400-13,230 pg/L) was higher than for Lake waters (range perfluorooctanoic acid 400-11,650 and perfluorooctane sulfonate <400-2,530 pg/L respectively) suggesting generalized point sources such as domestic and industrial waste.