A study on the behaviour of pesticides and their transformation products in the Scheldt estuary using liquid chromatography-electrospray tandem mass spectrometry

Off-line solid-phase extraction (SPE) combined with liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS-MS) was used to study the estuarine behaviour of the polar pesticides, atrazine, chloridazon, diuron and metolachlor, and their transformation products (TPs), hydroxyatrazine (HA), desisopropylatrazine (DIA), desethylatrazine (DEA), 3,4-dichlorophenylmethylurea (DPMU) and monuron. The compounds were identified by comparing their LC retention times and product-ion spectra with those of standard solutions. In all but one case the detection limits of the method were sufficient to determine the compounds of interest over the entire salinity range in the estuary. The concentrations of the dissolved pesticides ranged from 70 ng l-1 for chloridazon to 1350 ng l-1 for diuron. The levels of TPs were 3-8% of the levels of their parent pesticide. The mixing plots of polar pesticides and their TPs indicated that TPs, which are present in fresh river water, are conservatively transported to the sea and that no additional amounts of TPs are formed during their transport through the estuary. The one exception was HA, of which approximately 10% of the amount transported to the North Sea is formed in the lower part of the estuary by photochemical oxidation of atrazine. The latter was concluded from the ratios of each analyte over the sum total of the parent pesticide and all TPs along the salinity gradient, which proved to be a useful tool for identifying such estuarine transformations.     

The use of gas chromatography with ion-trap MS/MS detection for the determination of planar PCBs in biota and sediment

Combining capillary GC with ion-trap detection in the MS/MS mode allows the determination of trace levels of the highly toxic PCB congeners, CB 77, 126 and 169 in complex biological tissues, suspended matter and sediment. The high selectivity and sensitivity of MS/MS detection in the resonant and non-resonant modes yield detection limits of 60 fg, 300 fg and 200 fg for CB 77, 126, and 169, respectively.     

Polychlorinated biphenyls in marine sediments from the southern North Sea and Scheldt estuary: a ten-year study of concentrations, patterns and trends

The paper reports the concentrations and patterns of CBs in sediments of the Belgian part of the southern North Sea and the Scheldt estuary for the period 1991-2001. The long-term analytical performance was well within the quality assurance boundaries set at the outset of the study and is consistent with the state of the art for this type of analysis. The CB concentrations (given as the median of the sum of IUPAC Nos 28, 52, 101, 118, 138, 153 and 180) vary between 0.1 microg kg(-1) and 50 microg kg(-1) dry weight in the total sediment and it could be demonstrated that CB patterns in the fine fraction of the sediment were closely similar throughout the investigated area. Isolation of the fine fraction (<63 microm) by sieving can be regarded as a physical normalisation to reduce the differences in sediment granulometric composition. It allows for a better understanding of CB distribution and patterns and improves the trend analysis. A significant downward trend could not be found at any of the stations, which suggests that CB levels have not been changing in the area of interest in the past decade.     

环境中的药物——LC-MS/MS分析地表水和地下水

成百上千的活性物质正被用于人药和兽药处方中.由于药物的广泛应用,它们的残留物可通过多种途径进入环境.虽然主要通过尿和粪便的排泄,但是药品生产中的排放也应被考虑.当抗生素用于水产业,就会产生更直接的影响.污水处理设备不能完全除去药物,因此药物会出现在地表和地下水样品中.近年来,人们对环境中药物的兴趣正在增加,需要建立一种快速、灵敏、有选择性的方法来分析水样.     

Enantiomer fractions instead of enantiomer ratios

The use of enantiomer ratios (ERs) to indicate the relative amounts of a pair of enantiomers in a sample has some disadvantages. Enantiomer fractions (EFs) are proposed as an alternative expression to eliminate the difficulties.     

Determination of metoxuron and 3-chloro-4-methoxyaniline via direct derivatization with heptafluorobutyric anhydride and GC-ECD

The phenylurea herbicide metoxuron and its main metabolite, 3-chloro-4-methoxyaniline, can be determined rapidly in aqueous samples via extraction, derivatization with heptafluorobutyric anhydride (HFBA), washing with an aqueous bufferof pH 8, and analysis by capillary GC with electron capture detection. Linear calibration curves are obtained over two orders of magnitude, and the detection limit for the HFB derivatives is about 0.5 pg. The method has successfully been applied to several types of water samples.     

Source identification of personal exposure to fine particulate matter using organic tracers

Personal exposure to fine particulate matter (PM2.5) is due to both indoor and outdoor sources. Contributions of sources to personal exposure can be quite different from those observed at ambient sampling locations. The primary goal of this study was to investigate the effectiveness of using trace organic speciation data to help identify sources influencing PM2.5 exposure concentrations. Sixty-four 24-h PM2.5 samples were obtained on seven different subjects in and around Boulder, CO. The exposure samples were analyzed for PM2.5 mass, elemental and organic carbon, organic tracer compounds, water-soluble metals, ammonia, and nitrate. This study is the first to measure a broad distribution of organic tracer compounds in PM2.5 personal samples. PM2.5 mass exposure concentrations averaged 8.4 μg m^?3. Organic carbon was the dominant constituent of the PM2.5 mass. Forty-four organic species and 19 water-soluble metals were quantifiable in more than half of the samples. Fifty-four organic species and 16 water-soluble metals had measurement signal-to-noise ratios larger than two after blank subtraction.The dataset was analyzed by Principal Component Analysis (PCA) to determine the factors that account for the greatest variance. Eight significant factors were identified; each factor was matched to its likely source based primarily on the marker species that loaded the factor. The results were consistent with the expectation that multiple marker species for the same source loaded the same factor. Meat cooking was an important source of variability. The factor that represents meat cooking was highly correlated with organic carbon concentrations (r = 0.84). The correlation between ambient PM2.5 and PM2.5 exposure was relatively weak (r = 0.15). Time participants spent performing various activities was generally not well correlated with PCA factor scores, likely because activity duration does not measure emissions intensity. The PCA results demonstrate that organic tracers can aid in identifying factors that influence personal exposures to PM2.5.     

Contamination in sediments, bivalves and sponges of McMurdo Sound, Antarctica

This study examined the concentrations of total hydrocarbons (THC), polychlorinated biphenyls (PCB), polyaromatic hydrocarbons (PAH), and trace metals (Cu, Zn, Cd, Pb, Hg and As) in marine sediments off Scott Base (NZ) and compared them with sediments near the highly polluted McMurdo Station (US) as well as less impacted sites including Turtle Rock and Cape Evans. The Antarctic mollusc, Laternula elliptica and three common sponge species were also analysed for trace metals. The mean THC concentration in sediments from Scott Base was 3 fold higher than the pristine site, Turtle Rock, but 10 fold lower than samples from McMurdo Station. McMurdo Station sediments also contained the highest concentrations of PAHs, PCBs and the trace metals, Cu, Zn, Pb, Cd and Hg. Copper was significantly higher in bivalves from McMurdo Station than other sites. Trace metal concentrations in sponges were generally consistent within sites but no spatial patterns were apparent.     

Mass balance of trichloroacetic acid in the soil top layer

Since the ban on the use of trichloroacetic acid (TCAA) as a herbicide in several countries, TCAA is still found ubiquitously in the environment. The presence of TCAA nowadays is suggested to originate mainly from the atmospheric degradation of tetrachloroethene. Our mass balance calculations indicate that this may be true for the presence of TCAA in the atmosphere. However, our mass balance calculations also provide tentative evidence for the formation of TCAA in soil. If our calculated production fluxes are realistic estimates, a very large source of TCAA in soil has been identified.     

Comparison of methods for the extraction and determination of polychlorinated biphenyls in shiphull antifoulings

A method is presented for the determination of PCBs in chlorinated rubber antifoulings. In ten different brands, no PCB concentrations above 0.5 mg kg^?1 were found.