Reduced solvent and reagent amounts: effect on carbonyl dinitrophenylhydrazone measurements at low concentrations.

This work aims to advance towards a more affordable laboratory procedure for sample treatment to determine carbonyl compounds by derivatization with 2,4-dinitrophenylhydrazine (DNPH). The proposal is based on reducing the amount of DNPH and solvents. A simple addition of standard carbonyls in a solution containing DNPH to prepare hydrazone standards is described and evaluated. Tedious recrystallization steps are avoided. Formaldehyde, acetaldehyde, acetone, tolualdehyde and hexanal, as carbonyl models, were quantified using a DNPH concentration of 400 µg mL-1 and 3.8 mM H2SO4 and by keeping for 24 hours at room temperature. Analytical coefficients of variation between 10 and 25% were found from the analysis of blanks under intermediate conditions (two different devices, very different concentrations of DNPH and analysis on two days). From these values of relative standard deviations and background levels, quantification limits were estimated between 15 and 40 ng mL-1. The reduction of reagent amounts allows the operator to better control the background levels in the use of DNPH, as well as making the method more cost-effective and easy to use. In short, it leads to a more sustainable adaptation of the classical method. The versatility in analytical application was tested to estimate the levels of formaldehyde, acetaldehyde and acetone in very different types of environmental samples. In particular, outdoor and indoor samples were collected in filters and impregnated cartridges, respectively. Moreover, tars in 2-propanol and particulate matter from gasification processes were also tested.

Organic Analysis of Environmental Samples Using Liquid Chromatography with Diode Array and Fluorescence Detectors: An Overview.

This overview is focused to provide an useful guide of the families of organic pollutants that can be determined by liquid chromatography operating in reverse phase and ultraviolet/fluorescence detection. Eight families have been classified as the main groups to be considered: carbonyls, carboxyls, aromatics, phenols, phthalates, isocyanates, pesticides and emerging. The references have been selected based on analytical methods used in the environmental field, including both the well-established procedures and those more recently developed.

Validating Analytical Protocols to Determine Selected Pesticides and PCBs Using Routine Samples.

This study aims at providing recommendations concerning the validation of analytical protocols by using routine samples. It is intended to provide a case-study on how to validate the analytical methods in different environmental matrices. In order to analyze the selected compounds (pesticides and polychlorinated biphenyls) in two different environmental matrices, the current work has performed and validated two analytical procedures by GC-MS. A description is given of the validation of the two protocols by the analysis of more than 30 samples of water and sediments collected along nine months. The present work also scopes the uncertainty associated with both analytical protocols. In detail, uncertainty of water sample was performed through a conventional approach. However, for the sediments matrices, the estimation of proportional/constant bias is also included due to its inhomogeneity. Results for the sediment matrix are reliable, showing a range 25-35% of analytical variability associated with intermediate conditions. The analytical methodology for the water matrix determines the selected compounds with acceptable recoveries and the combined uncertainty ranges between 20 and 30%. Analyzing routine samples is rarely applied to assess trueness of novel analytical methods and up to now this methodology was not focused on organochlorine compounds in environmental matrices.

An evaluation of uncertainty associated to analytical measurements of selected polycyclic aromatic compounds in ambient air.

This paper presents an evaluation of uncertainty associated to analytical measurement of 18 polycyclic aromatic compounds (PACs) in ambient air by liquid chromatography with fluorescence detection (HPLC/FD). The study was focused on analyses of PM(10), PM(2.5) and gas phase fractions. Main analytical uncertainty was estimated for 11 polycyclic aromatic hydrocarbons (PAHs), four nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) and two hydroxy-polycyclic aromatic hydrocarbons (OH-PAHs) based on the analytical determination, reference material analysis and extraction step. Main contributions reached 15-30% and came from extraction process of real ambient samples, being those for nitro-PAHs the highest (20-30%). Range and mean concentration of selected PACs measured in gas phase and PM(10)/PM(2.5) particle fractions during a full year are also presented. Concentrations of OH-PAHs were about 2-4 orders of magnitude lower than their parent PAHs and comparable to those sparsely reported in literature.

Assessment uncertainty associated to the analysis of organic compounds linked to particulate matter of atmospheric aerosols.

Current work has evaluated uncertainty associated to quantification of several organic compounds present in particulate matter of atmospheric aerosols, setting out the stages of analytical procedure that contribute most to the global uncertainty. Several sources of uncertainty have been identified, which were clustered into five main contributions: sampling, extraction, clean-up, derivatization and analysis. A discussion of the main contributions to the overall uncertainty is reported, allowing authors to locate the largest ones and plan future improvements. Combined uncertainties ranged between 10-18% (alkanes), 12-16% (PAHs), 10-18% (alcohols) and 9-21% (acids). The analytical procedure was validated by analysing a standard reference material (SRM1649a, urban dust). Also, the proposed method was applied to the analysis of four samples of particulate matter.

Large Evaluation of Anti-Cardiolipin and anti-Beta2Glycoprotein I Assays: Results from the AutoimmunityWorkshop of the Spanish Society of Immunology

Despite their clinical utility and the importance that laboratory testshave in APS diagnosis, probably the most important drawback of suchtests is the elevated intra- and inter-laboratory variation. The aim of thepresent work was to assess the multilaboratory performance of aCL (..) (AU)

A pesar de la indudable utilidad clínica y de la importancia de laspruebas de laboratorio en el diagnóstico del síndrome antifosfolípido(APS), probablemente el mayor defecto de dichas pruebas es su elevadavariabilidad intra- e inter-laboratorio. El objetivo del presente trabajo fueevaluar el comportamiento de los ensayos (..) (AU)