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901.
Mira Petrovic Marinella Farré Miren Lopez de Alda Sandra Perez Cristina Postigo Marianne Köck Jelena Radjenovic Merixell Gros Damia Barcelo 《Journal of chromatography. A》2010,1217(25):4004-4017
An overview of liquid chromatography–mass spectrometry methods used for the determination of trace organic contaminants in environmental samples is presented. Among the organic contaminants the focus is given on five groups of emerging contaminants that raised most concern as environmental contaminants and therefore attracted attention of a research community: pharmaceuticals, drugs of abuse, polar pesticides, perfluorinated compounds and nanoparticles. Various aspects of current LC–MS methodology, using tandem and hybrid MS instruments, including sample preparation, are discussed. 相似文献
902.
Bienvenida Gilbert-López Juan F. García-Reyes Ana Lozano Amadeo R. Fernández-Alba Antonio Molina-Díaz 《Journal of chromatography. A》2010,1217(39):6022-6035
In this work we have evaluated the performance of two sample preparation methodologies for the large-scale multiresidue analysis of pesticides in olives using liquid chromatography–electrospray tandem mass spectrometry (LC–MS/MS). The tested sample treatment methodologies were: (1) liquid–liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using GCB, PSA and C18 sorbents (QuEChERS method – modified for fatty vegetables) and (2) matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a final clean-up performed in the elution step using Florisil. An LC–MS/MS method covering 104 multiclass pesticides was developed to examine the performance of these two protocols. The separation of the compounds from the olive extracts was achieved using a short C18 column (50 mm × 4.6 mm i.d.) with 1.8 μm particle size. The identification and confirmation of the compounds was based on retention time matching along with the presence (and ratio) of two typical MRM transitions. Limits of detection obtained were lower than 10 μg kg−1 for 89% analytes using both sample treatment protocols. Recoveries studies performed on olives samples spiked at two concentration levels (10 and 100 μg kg−1) yielded average recoveries in the range 70–120% for most analytes when QuEChERS procedure is employed. When MSPD was the choice for sample extraction, recoveries obtained were in the range 50–70% for most of target compounds. The proposed methods were successfully applied to the analysis of real olives samples, revealing the presence of some of the target species in the μg kg−1 range. Besides the evaluation of the sample preparation approaches, we also discuss the use of advanced software features associated to MRM method development that overcome several limitations and drawbacks associated to MS/MS methods (time segments boundaries, tedious method development/manual scheduling and acquisition limitations). This software feature recently offered by different vendors is based on an algorithm that associates retention time data for each individual MS/MS transition, so that the number of simultaneously traced transitions throughout the entire chromatographic run (dwell times and sensitivity) is maximized. 相似文献
903.
Hannah Runnqvist Søren Alex BakMartin Hansen Bjarne StyrishaveBent Halling-Sørensen Erland Björklund 《Journal of chromatography. A》2010,1217(16):2447-2470
Pressurised liquid extraction (PLE) is now a well established and extensively applied extraction technique in environmental analysis for pollutants such as persistent organic pollutants (POPs). During the past decade, an emerging group of environmentally interesting analytes are pharmaceuticals that are continuingly released into the environment. This class is comprised with compounds of various properties. As the field of the analysis of these compounds grows, an increasing number of PLE methods for pharmaceuticals of varying quality are developed and published. This review summarises the critical PLE parameters during PLE method development and highlight them with examples from recently published papers utilising pressurised liquid extraction for the determination of pharmaceuticals in environmental and biological matrices. These recent methods are summarised and critically discussed with the aim to provide important reflections to alleviate in future PLE development for pharmaceuticals in environmental matrices. 相似文献
904.
从铅中毒发铅诊断标准、发铅诊断试验及发铅诊断临床应用3个方面论述了发铅检测法在铅中毒诊断、筛查和监督中的实际应用问题。根据临床经验和发铅-血铅比值确定了居民发铅正常值上限及铅中毒发铅诊断分级标准;即使以血铅测定值为"金标准",诊断试验表明,发铅测定在铅中毒诊断中仍有实际应用价值;发铅检测法自上世纪60年代以来一直沿用至今,绝大多数研究者认为,发铅测定是诊断、筛查铅中毒和监督环境铅污染最简单、有效的工具。 相似文献
905.
A simple, cheap and flexible flowcell based on a standard 5 mm NMR tube, designed for the monitoring of reactions but of wide applicability, is described. No modification of the NMR instrument is needed, allowing the system to be employed with any conventional NMR probe and magnet. The system is robust and economical in use of reagents, and can be used for studying both homogeneous and heterogeneous reactions. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
906.
An overview of sample preparation and extraction of synthetic pyrethroids from water,sediment and soil 总被引:1,自引:0,他引:1
Saeed S. Albaseer R. Nageswara Rao Y.V. Swamy K. Mukkanti 《Journal of chromatography. A》2010,1217(35):5537-5554
The latest developments in sample preparation and extraction of synthetic pyrethroids from environmental matrices viz., water, sediment and soil were reviewed. Though the synthetic pyrethroids were launched in 1970s, to the best of authors’ knowledge there was no review on this subject until date. The present status and recent advances made during the last 10 years in sample preparation including conservation and extraction techniques used in determination of synthetic pyrethroids in water, sediment and soil were discussed. Pre- and post-extraction treatments, sample stability during extraction and its influence upon the whole process of analytical determination were covered. Relative merits and demerits including the green aspects of extraction were evaluated. The current trends and future prospects were also addressed. 相似文献
907.
《Biomedical chromatography : BMC》2017,31(10)
A simple, accurate and selective column‐switching high‐performance liquid chromatography (HPLC) method was developed and validated for simultaneous quantification of six beta ‐blockers (metoprolol, timolol, bisoprolol, propranolol, carvedilol and nebivolol), three of their metabolites (α ‐hydroxy metoprolol, N‐ desisopropyl propranolol and 4′‐hydroxy carvedilol 4‐HCAR), three antipsychotics (olanzapine, clozapine and quetiapine) and three of their metabolites (N‐ desmethyl olanzapine, N‐ desmethyl clozapine and N‐ desalkyl quetiapine) in human serum. After pretreatment on a Merck LiChrospher RP‐4 ADS column (25 μm), drugs were separated on a Phenomenex Gemini Phenyl Hexyl 110 A column (250 × 4.6 mm, 5 μm) using a gradient mixture of acetonitrile and potassium dihydrogen phosphate buffer pH 3.1 (containing 10% methanol) as a mobile phase at a flow rate of 1 mL/min. The total analysis time was 40 min. For detection of the analytes, four different UV wavelengths were used: 215, 226, 242 and 299 nm. The method was validated according to the guidelines of the Society of Toxicology and Forensic Chemistry in terms of selectivity, linearity, accuracy, precision and stability and successfully applied for the analysis of the 15 described analytes in human serum. 相似文献
908.
Due to recent advances in passive acoustic monitoring techniques, beaked whales are now more effectively detected acoustically than visually during vessel-based (e.g. line-transect) surveys. Beaked whales signals can be discriminated from those of other cetaceans by the unique characteristics of their echolocation clicks (e.g. duration >175 μs, center frequencies between 30 and 40 kHz, inter-click intervals between 0.2 and 0.4 s and frequency upsweeps). Furthermore, these same characteristics make these signals ideal candidates for testing automated detection and classification algorithms. There are several different beaked whale automated detectors currently available for use. However, no comparative analysis of detectors exists. Therefore, comparison between studies and datasets is difficult. The purpose of this study was to test, validate, and compare algorithms for detection of beaked whales in acoustic line-transect survey data. Six different detection algorithms (XBAT, Ishmael, PAMGUARD, ERMA, GMM and FMCD) were evaluated and compared. Detection trials were run on three sample days of towed-hydrophone array recordings collected by NOAA Southwest Fisheries Science Center (SWFSC) during which were confirmed visual sightings of beaked whales (Ziphius cavirostris and Mesoplodon peruvianus). Detections also were compared to human verified acoustic detections for a subset of these data. In order to measure the probabilities of false detection, each detector was also run on three sample recordings containing clicks from another species: Risso’s dolphin (Grampus griseus). Qualitative and quantitative comparisons and the detection performance of the different algorithms are discussed. 相似文献
909.
Riyad Ahmed Al-Okab 《Talanta》2007,72(4):1239-1247
Nine spectrophotometric methods based on new reactions for the determination of tracer amounts of nitrite in environmental samples were developed. Replacement of toxic reagents was explored to attain the standards of clean chemistry. These methods utilize two classes of compounds namely; phenoxazines and sulphonamides, the well established drugs in the presence of limited amounts of hydrochloric acid. The methods were based on the oxidation of sulfanilamide (SAA), sulfadoxine (SDX) or sulfamethoxazole (SMX) by nitrite in hydrochloric acid medium and coupling with phenoxazine (PNZ), 2-chlorophenoxazine (CPN) or 2-trifluoromethylphenoxazine (TPN) which yielded red colored derivatives having an absorbance maximum in the range 530-540 nm and were stable for about 4 h. Beer's law was obeyed for nitrite in the concentration range 0.13-1.60 μg mL−1. The reaction conditions and other important analytical parameters were optimized to enhance the sensitivity of the methods. Interference if any, by non-target ions was also investigated. The methods were applied determining nitrite in environmental samples. The performance of these methods were evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference spectrophotometric method. 相似文献
910.
Daniel Lumpi Christian Hametner Bernhard Zachhuber Johannes Fröhlich 《Tetrahedron letters》2009,50(47):6469-6471
A convenient approach for the synthesis of monodisperse oligo(ethylene glycols) up to 12 units is described. A novel cleavage protocol replacing laborious hydrogenolysis is introduced to achieve a fast, inexpensive and widely applicable procedure. In addition to the synthetic part, Fourier transform infrared (FTIR) spectroscopy using a fibre optic attenuated total reflection (ATR) sensor was applied to monitor the formation of sensitive key intermediates, resulting in optimized reaction times. By applying this in-line technique, the possibility of real-time analysis under inert conditions was impressively demonstrated. 相似文献