Determination of metals in thoracic fraction of ambient air particulate matter

The present work deals with the optimization and validation of a method for the quantitative simultaneous ICP determination of metals in ambient air particulate matter. The attention has been focused on the thoracic fraction (PM10) and twelve different metals were chosen on the basis of their toxicity and of their possible use as chemical tracers. The microwave acidic digestion of the samples has been performed in the presence of different reagents and under different conditions and particular attention has been paid to the optimization of the whole analytical procedure and to the evaluation of accuracy and precision related to the single operative steps. The interferences due to the reagents and to the sampling supports have also been evaluated. In addition, the analytical procedure has been checked by examining the equivalence of results related to parallel sampled filters pairs.     

Synthesis and crystal structure of unprecedented phosphine adducts of d(1)-aryl imido-vanadium(IV) complexes

The reaction of the imido precursor [V(NAr)Cl(2)](n)() (1) (Ar = 2,6-i-Pr(2)C(6)H(3)) with 3 equiv of PMe(2)Ph yields the monomeric complex [V(=NAr)Cl(2)(PMe(2)Ph)(2)] (2). Reacting 1 with 1.5 equiv of dmpe or 1 equiv of dppm affords the dimeric complexes [V(=NAr)Cl(2)(dmpe)](2)(mu-P,P'-dmpe) (3) and [V(=NAr)Cl(2)(dppm)](2) (4), respectively. Complexes 2-4 have been fully characterized by spectroscopic methods, magnetism studies, and X-ray crystallography.     

Synthesis of a new solid-phase extractor and its application to preconcentration and determination of lead in water samples

A procedure for preconcentration and determination of lead in water is described. The method is based on the sorption of Pb(II) in a minicolumn packed with a functionalized sorbent and subsequent elution with acidic solution. The determination of lead content in the eluate was carried out using flame atomic absorption spectrometry. The sorbent was prepared by immobilization of the ligand 4-(5'-bromo-2'-thiazolylazo)orcinol on polystyrene-divinylbenzene through an azo spacer. Diazotization and coupling reactions were used for synthesis of the sorbent. Some variables affecting the preconcentration were optimized using a full factorial design. Under optimized conditions, the method presented a detection limit of 0.5 microg/L and enrichment factor of 36 for a sample volume of 25 mL. The accuracy of the method was tested by the determination of lead in a standard reference material (National Institute of Standards and Technology 1643d Fresh Water). The proposed procedure was applied to the determination of lead in samples of natural and drinking waters.     

Essential oils of Daucus carota subsp. carota of Tunisia obtained by supercritical carbon dioxide extraction

The essential oils and supercritical CO2 extracts of wild Daucus carota L. subsp. carota from two different sites in Tunisia were investigated. The main components of the essential oil of the flowering and mature umbels with seeds from Sejnane were eudesm-7(11)-en-4-ol (8.2 - 8.5%), carotol (3.5 - 5.2%), sabinene (12.0 -14.5%), a-selinene (7.4 - 8.6) and 11-alpha-(H)-himachal-4-en-1-beta-ol (12.7 - 17.4%), whereas the oils from Tunis were predominantly composed of elemicin (31.5 - 35.3%) and carotol (48.0 - 55.7%). The antimicrobial activity of the essential oils were assayed by using the broth dilution method on Escherichia coli ATCC 35218 and Staphylococcus aureus ATCC 43300, and clinical strains of Candida albicans and C. tropicalis 1011 RM. The MIC values obtained were all > 2.5% (v/v).     

Chemical constituents and larvicidal activity of Hymenaea courbaril fruit peel

The chemical compositions of the essential oils from the peel of ripe and unripe fruits of Hymenaea courbaril L., obtained by hydrodistillation, were analyzed by GC and GC-MS. The main constituents of the essential oil from the peel of the ripe fruits were the sesquiterpenes alpha-copaene (11.1%), spathulenol (10.1%) and beta-selinene (8.2%), while germacrene-D (31.9%), beta-caryophyllene (27.1%) and bicyclogermacrene (6.5%) were the major compounds in the oil from unripe fruits. The essential oils were tested against Aedes aegypti larvae and showed LC50 values of 14.8 +/- 0.4 microg/mL and 28.4 +/- 0.3 microg/mL for the ripe and unripe fruit peel oils, respectively. From the peel of the ripe fruits, the diterpenes zanzibaric acid and isoozic acid were isolated, along with the sesquiterpene caryolane-1,9beta-diol. To the best of our knowledge, this is the first report of this sesquiterpene in the genus. The structures of all compounds isolated were identified on the basis of their spectral data (IR, MS, 1D- and 2D-NMR) and by comparison with literature spectral data.     

Volatile components of Centaurea bracteata and C. pannonica subsp. pannonica growing wild in Croatia

This paper reports on the volatile components of oils from the aerial parts (CBA) and roots (CBR) of Centaurea bracteata Scop. and aerial parts of C. pannonica (Heuffel) Simonkai subsp. pannonica (CPA), two Asteraceae growing wild in Croatia. The volatile components, obtained by hydrodistillation, were determined by GC-MS analysis. The yields (w/w) of the dried oils were 0.10% (CBA), 0.22% (CBR) and 0.09% (CPA), respectively. A total of 91 compounds were identified accounting for 91.1%, 93.3% and 87.9% of the total oil for CBA, CBR and CPA, respectively. All the samples were characterized mainly by hydrocarbons (7.1-34.1%), fatty acids (9.7-45.9%), and oxygenated sesquiterpenes (15.2-16.6%). The major components of the samples were hexadecanoic acid (8.1-31.1%), nonacosane (0.6-13.4%) and caryophyllene oxide (4.5-11.9%). Monoterpenes, both hydrocarbons and oxygenated, were either absent or present in low amounts in all the oils. The similarity in the oil contents is consistent with the two species being placed in the same section, Jacea.     

Polymeric Multilayer Capsules in Drug Delivery

Recent advances in medicine and biotechnology have prompted the need to develop nanoengineered delivery systems that can encapsulate a wide variety of novel therapeutics such as proteins, chemotherapeutics, and nucleic acids. Moreover, these delivery systems should be “intelligent”, such that they can deliver their payload at a well‐defined time, place, or after a specific stimulus. Polymeric multilayer capsules, made by layer‐by‐layer (LbL) coating of a sacrificial template followed by dissolution of the template, allow the design of microcapsules in aqueous conditions by using simple building blocks and assembly procedures, and provide a previously unmet control over the functionality of the microcapsules. Polymeric multilayer capsules have recently received increased interest from the life science community, and many interesting systems have appeared in the literature with biodegradable components and biospecific functionalities. In this Review we give an overview of the recent breakthroughs in their application for drug delivery.     

New advances in method validation and measurement uncertainty aimed at improving the quality of chemical data

The implementation of quality systems in analytical laboratories has now, in general, been achieved. While this requirement significantly modified the way that the laboratories were run, it has also improved the quality of the results. The key idea is to use analytical procedures which produce results that fulfil the users needs and actually help when making decisions. This paper presents the implications of quality systems on the conception and development of an analytical procedure. It introduces the concept of the lifecycle of a method as a model that can be used to organize the selection, development, validation and routine application of a method. It underlines the importance of method validation, and presents a recent approach based on the accuracy profile to illustrate how validation must be fully integrated into the basic design of the method. Thanks to the -expectation tolerance interval introduced by Mee (Technometrics (1984) 26(3):251–253), it is possible to unambiguously demonstrate the fitness for purpose of a new method. Remembering that it is also a requirement for accredited laboratories to express the measurement uncertainty, the authors show that uncertainty can be easily related to the trueness and precision of the data collected when building the method accuracy profile.     

Quality assurance and quality control in forest soil analyses: a comparison between European soil laboratories

In transnational monitoring programmes, a balance between international reference methods, which improve spatial comparability, and national analysis methods that favour temporal comparability, by their use and testing over many years, needs to be sought. Prior to the next Pan-European Forest Soil Survey, a third interlaboratory comparison of soil analysis methods was organised. All participating laboratories were requested to use the same reference methods. Fifty-two soil laboratories from 27 European countries analysed a total of 48 soil parameters on three soil samples which were typical for European forest soils. The results of the statistical analysis showed a high interlaboratory and intralaboratory variability, especially for the acid oxalate extractions, particle size distribution, exchangeable elements and total carbonates. The intercomparability of the test results did not improve compared to the previous ring test. As the exercise aimed primarily at comparing the performance of the laboratories, it was not powerful enough to find cause–effect relationships between the meta information provided by the laboratories and the variability of the test results.