Search results for "solid phase"
showing 10 items of 360 documents
An automatic flow-through system for exploration of the human bioaccessibility of endocrine disrupting compounds from microplastics
2021
This article reports on the first attempt towards investigating the leaching rates in the human gastrointestinal (GI) tract of plastic-borne contaminants that can be ingested accidentally using physiologically relevant body fluids. Oral bioaccessibility under fasted and fed states was determined in dynamic mode exploiting an automatic flow setup. The flow system is able to mimic the fast uptake of the released species from the polymeric matrix by absorption in the human digestive system by the in-line removal of the leached species. Complex GI extractants based on the Unified Bioaccessibility Method (UBM, fasted state) and Versantvoort test (fed-state) were brought through a microplastic-lo…
Investigation of sterols as potential biomarkers for the detection of pig (S. s. domesticus) decomposition fluid in soils
2012
This study was carried out to evaluate the potential of using cholesterol and coprostanol, as indicators for the detection of decomposition fluid of buried pigs (S. s. domesticus) in soils. In May 2007, four pig carcasses (~35. kg) were buried in shallow graves (~40. cm depth) at the University of Ontario Institute of Technology in Canada. Two pigs were exhumed after three months (Pig 1, Pig 2) and six months (Pig 3, Pig 4) post burial. Soil samples were collected beneath the pig carcasses (~40. cm depth) and from grave walls (~15-20. cm depth) as well as from a parallel control site. Coprostanol and cholesterol were extracted from soils, purified with solid phase extraction (SPE) and analy…
Simultaneous determination of eight underivatised biogenic amines in fish by solid phase extraction and liquid chromatography-tandem mass spectrometr…
2010
Biogenic amines on fish tissue are formed as a result of bacterial contamination and spoilage during storage. A new method based on liquid chromatography (LC) and tandem mass spectrometry (MS/MS) using a triple quadrupole (QqQ) analyser was developed for the analysis of eight biogenic amines (cadaverine, histamine, phenylethylamine, putrescine, spermine, spermidine, tyramine and tryptamine) in fish tissues. Sample preparation was performed by extraction with trichloroacetic acid 5% and solid phase extraction clean up with STRATA X cartridge. The MS/MS method was validated and compared with a method based on the analysis of dansyl derivatives by LC and fluorescence detector (FD). MS/MS achie…
In-situ suspended aggregate microextraction: A sample preparation approach for the enrichment of organic compounds in aqueous solutions.
2015
Abstract This work presents in-situ suspended aggregate microextraction (iSAME) as a new and expedient sample preparation method. This new concept capitalizes on the general principles of in-situ solvent formation microextraction, in the sense that extraction is carried out in a supramolecular aggregate phase, which is formed in-situ in the sample through one-step process involving ion-association between a cationic surfactant and a benzene sulfonic acid derivative. The suspended aggregate containing the analytes is then collected in the form of a thin-film on the surface of a common filter paper by suction filtration. The entrapped analytes are released by completely dissolving the thin-fi…
An automated and self-cleaning nano liquid chromatography mass spectrometry platform featuring an open tubular multi-hole crystal fiber solid phase e…
2017
An open tubular (OT) sample preparation/separation platform was developed. A multi-channel polymer layer open tubular (mPLOT) solid phase extraction (SPE) column was prepared by wall-coating the 126 channels (8μm inner diameter (ID) each) of a crystal fiber capillary with an organic polymer, namely poly(styrene-co-octadecene-co-divinylbenzene) (PS-OD-DVB). The mPLOT SPE was coupled on-line with a 10μm×2m poly(styrene-co-divinylbenzene) (PS-DVB) OT liquid chromatography column with nanospray mass spectrometry (OTLC-MS). Compared to using monolithic/particle-packed SPEs, mPLOT-SPE-OTLC allowed both fast loading and sufficient refocusing on the OT analytical column of small model compounds (su…
Ion-pair in-tube solid-phase microextraction and capillary liquid chromatography using a titania-based column: application to the specific lauralkoni…
2012
Abstract A quick, miniaturized and on-line method has been developed for the determination in water of the predominant homologue of benzalkonium chloride, dodecyl dimethyl benzyl ammonium chloride or lauralkonium chloride (C 12 -BAK). The method is based on the formation of an ion-pair in both in-tube solid-phase microextraction (IT-SPME) and capillary liquid chromatography. The IT-SPME optimization required the study of the length and nature of the stationary phase of capillary and the processed sample volume. Because to the surfactant character of the analyte both, the extracting and replacing solvents, have played a decisive role in the IT-SPME optimized procedure. Conditioning the capil…
Recent Advances in Sample Preparation for Pesticide Analysis
2012
Much progress has been made in pesticide analysis in the past decade. During this time, hyphenated techniques involving highly efficient separation with sensitive mass spectrometric detection have become the methods of choice. Even with such powerful instrumental techniques, a demanding task in pesticide residue analysis is the development of multiresidue methods for the determination of pesticides in air, water, soil, sediment, biota, and food. This chapter summarizes the analytical characteristics of the different methods of sample preparation for the determination of pesticide residues in a variety of food matrices, and surveys their recent applications in combination with gas chromatogr…
Solid-Phase Extraction and Clean-Up Procedures in Pharmaceutical Analysis
2012
Solid-phase extraction (SPE) using small cartridges filled with sorbents of a small particle size has rapidly established itself as an important sample clean-up technique. It has prospered at the expense of liquid-liquid extraction (LLE), which is considered labor intensive and frequently plagued by problems, such as emulsion formation and use of large volumes of hazardous solvents. A remarkable characteristic of SPE is its easy adaptation to on-line mode by column-switching techniques; switching can be effected manually or by automated controllers. The same analyte/sorbent interactions that are exploited in liquid chromatography (LC) are of use in SPE, but particle sizes employed are great…
Formation of the C−S−H Layer during Early Hydration of Tricalcium Silicate Grains with Different Sizes
2005
Portland cement is a mixture of solid phases which all react with water. Tricalcium silicate (Ca3SiO5) is its main component and is often used in model systems to study cement hydration. It is generally recognized that setting and hardening of cement are due to the formation, by a dissolution-precipitation process, of a calcium silicate hydrate (C-S-H) on anhydrous grains during Ca3SiO5 hydration. The purpose of this paper is to study the effect of Ca3SiO5 particle size on the nucleation-growth process of C-S-H. An experimental study of the rate of hydration by using different grain sizes under controlled conditions has been performed. The experimental data have been compared with results o…
Extraction of uranyl ions from aqueous solutions using silica-gel-bound macrocycles for alpha contaminated waste water treatment
2004
Abstract The efficiency for the extraction of U(VI) of new modified silica gels, namely N-tripropionate (or N-triacetate)-substituted tetraazamacrocycles-bound silica gels, has been studied. The effect of the nature of the ligand, the pH and the temperature was studied both in batch experiments as well as in continuous extraction. These silica gels are good candidates for the extraction of U(VI) when compared to a commercially available acid-type chelating resin. The breakthrough and regeneration tests showed that the total removal of U(VI) from a contaminated solution can be achieved by using a column packed with such tetraazamacrocycles-bound silica gels. Finally, the use of a modified si…