Sampling in chemical analysis

The uncertainty of any analytical determination depends on analysis and sampling. Uncertainty arising from sampling is usually not controlled and methods for its evaluation are still little known. Pierre Gy’s sampling theory is currently the most complete theory about samplingwhich also takes the design of the sampling equipment into account. Guides dealing with the practical issues of sampling also exist, published by international organizations such as EURACHEM, IUPAC (International Union of Pure and Applied Chemistry) and ISO (International Organization for Standardization). In this work Gy’s sampling theory was applied to several cases, including the analysis of chromite concentration estimated on SEM (Scanning Electron Microscope) images and estimation of the total uncertainty of a drug dissolution procedure. The results clearly show that Gy’s sampling theory can be utilized in both of the above-mentioned cases and that the uncertainties achieved are reliable. Variographic experiments introduced in Gy’s sampling theory are beneficially applied in analyzing the uncertainty of auto-correlated data sets such as industrial process data and environmental discharges. The periodic behaviour of these kinds of processes can be observed by variographic analysis as well as with fast Fourier transformation and auto-correlation functions. With variographic analysis, the uncertainties are estimated as a function of the sampling interval. This is advantageous when environmental data or process data are analyzed as it can be easily estimated how the sampling interval is affecting the overall uncertainty. If the sampling frequency is too high, unnecessary resources will be used. On the other hand, if a frequency is too low, the uncertainty of the determination may be unacceptably high. Variographic methods can also be utilized to estimate the uncertainty of spectral data produced by modern instruments. Since spectral data are multivariate, methods such as Principal Component Analysis (PCA) are needed when the data are analyzed. Optimization of a sampling plan increases the reliability of the analytical process which might at the end have beneficial effects on the economics of chemical analysis,

Passeig per l’invisible: itinerari químic per la ciutat de Girona = A walk through the invisible: a chemical journey through Girona

The presented itinerary covers eleven sites of the city of Girona that have been chosen for their interest from a chemical point of view. Girona is a city with chemistry, and this journey allowed student to see that chemistry is present everywhere, even in everyday life and not only in classrooms and laboratories. This approach aims to motivate students to discover something that had been invisible

Interleukin-4 induced leukocyte differentiation

Monocytes, macrophages and dendritic cells (DCs) are important mediators of innate immune system, whereas T lymphocytes are the effector cells of adaptive immune responses. DCs play a crucial role in bridging innate and adaptive immunity. Naïve CD4+ Th progenitors (Thp) differentiate to functionally distinct effector T cell subsets including Th1, Th2 and Th17 cells, which while being responsible for specific immune functions have also been implicated in pathological responses, such as autoimmunity, asthma and allergy. The main objective of this thesis is to dissect the signalling networks involved in the IL-4 induced differentiation of two important leukocyte subtypes, Th2 cells and DCs. Gene expression profiling lead to identification of over 200 genes which are differentially expressed during cytokine induced differentiation of human monocytes to DCs or macrophages and which are likely to be essential for the proper biological functions of these cell types. Transcriptome analysis demonstrated the dynamic regulation of gene expression by IL-12 and IL-4 during the initiation of Th cell differentiation, which was partly counteracted by an immunosuppressive cytokine, TGFβ, present in the culture media. Results from RNAi mediated gene knockdown experiments and global gene expression analysis elucidated that SATB1 regulates multiple genes important for Th cell polarization or function as well as may compete with GATA3 for the reciprocal regulation of IL-5 transcription. In conclusion, the results obtained have extended our system-level understanding of the immune cell differentiation processes and provide an excellent basis for the further functional studies which could lead to development of improved therapeutic approaches for a range of immunological conditions.

Chemical composition and antimicrobial activity of the essential oil of Hyptis pectinata (l.) Poit.

Essential oil was extracted from leaves of Hyptis pectinata using hydrodistillation, and its composition determined using GC-FID and GC-MS. Chemical analysis showed that there was a predominance of sesquiterpenes, of which β-caryophyllene (18.34%), caryophyllene oxide (18.00%) and calamusenone (24.68%) were measured for the first time in the genus Hyptis. Twenty-one compounds were identified, and calamusenone was isolated using preparative thin layer chromatography with a silica gel plate (60 PF254). The minimal inhibitory concentration (MIC) and minimal microbicidal concentration (MMC) were determined for various pathogenic microorganisms. H. pectinata oil was most effective against Gram (+) bacteria and yeasts.

Chemical composition and analgesic activity of the leaves and branches of Marlierea tomentosa Camb.

This paper describes the isolation of five phytoconstituents from Marlierea tomentosa. The triterpenes α-amyrin (1) and β-amyrin (2), and the flavonoids quercitrin (3) and isoquercetin (4), were isolated from the leaves. The branches afforded the triterpene arjunolic acid (5). The antinociceptive activity of crude extract, fractions and compound 5 were tested using the writhing and formalin tests in mice. The crude extract, some fractions, particularly dichloromethane and butanol (leaves), ethyl acetate (branches) and arjunolic acid (5) (81.2% inhibition) were more active against the writhing test than the two reference drugs, acetylsalicylic acid and indomethacin.

Constituintes químicos do caule de Senna reticulata Willd. (Leguminoseae): Chemical constituents isolated from the wood of Senna reticulata Willd.

The phytochemical investigation of the wood extracts of Senna reticulata (Leguminoseae) yielded six anthraquinones: chrysophanol, physcion, aloe-emodin, 1,3,8-trihydroxyanthraquinone, 3-methoxy-1,6,8-trihydroxyanthraquinone, emodin and the chrysophanol-10,10' bianthrone. The triterpenes a and b-amirin, the steroids b-sitosterol and stigmasterol as well as the flavonoid kaempferol were also identified. The structures were established by spectral analysis, including two-dimensional NMR techniques. It is the first report of 1,3,8-trihydroxyanthraquinone and 3-methoxy-1,6,8-trihydroxyanthraquinone in higher plants.

Avaliação da pós-graduação da área de química na CAPES e a internacionalização das revistas da Sociedade Brasileira de Química: Journal of the Brazilian Chemical Society e Química Nova

This paper discusses of the use of the Impact Factor in the evaluation of chemistry graduate courses by CAPES and the internationalization of the Journal of the Brazilian Chemical Society and Química Nova.

Productivity, Technical eficiency and internationalisation of the Spanish chemical sector

relationship between productivity and international position of Spanish chemical firms in the period 2005-2011. The goal is to determine whether companies that follow and international strategy, either with exports or by investment in foreign countries obtain greater productivity growth than these that do not operate in global market. For this purpose a panel data set with microdata has been created. A preliminary analysis of the evolution of productivity growth in the sector is carried out. The measurement of Total Factor Productivity is performed. With the estimated TFP we analyze the differentials in productivity growth, comparing the effects of export and investment behavior with non-international firms.

Chemical composition and antibacterial activities from the essential oils of myrtaceae species planted in Brazil

The essential oils of seven Myrtaceae species were investigated for its chemical composition and antibacterial activity. The volatile oils were characterized by a high content of monoterpenoids of which 1,8-cineole (88.0, 65.0 and 77.0% for Melaleuca hypericifolia, Callistemon viminalis and Callistemon citrinus respectively), terpinen-4-ol (47.0 and 49.8% for Melaleuca thymifolia and Callistemon polandii respectively) and α-pinene (54.5% for Kunzea ericoides) were the major components. The oil from M. linariifolia was characterized by a high concentration of methyleugenol (87.2%). The oil from Melaleuca thymifolia was the most active, exhibiting high antimicrobial activity against all tested bacteria.

pH effect on the synthesis of magnetite nanoparticles by the chemical reduction-precipitation method

This work aimed at putting in evidence the influence of the pH on the chemical nature and properties of the synthesized magnetic nanocomposites. Saturation magnetization measurements evidenced a marked difference of the magnetic behavior of samples, depending on the final pH of the solution after reaction. Magnetite and maghemite in different proportions were the main magnetic iron oxides actually identified. Synthesis with final pH between 9.7-10.6 produced nearly pure magnetite with little or no other associated iron oxide. Under other synthetic conditions, goethite also appears in proportions that depended upon the pH of the synthesis medium.

Perfil químico de cultivares de feijão (phaseolus vulgaris) pela técnica de high resolution magic angle spinning (HR-MAS)

The application of one-dimensional proton high-resolution magic angle spinning (¹H HR-MAS) NMR combined with a typical advantages of solid and liquid-state NMR techniques was used as input variables for the multivariate statistical analysis. In this paper, different cultivars of beans (Phaseolus vulgaris) developed and in development by Embrapa - Arroz e Feijão were analyzed by ¹H HR-MAS, which have been demonstrated to be a valuable tool in its differentiation according chemical composition and avoid the manipulation of the samples as used in other techniques.

Chemical constituents of Salacia elliptica (Celastraceae)

The chemical investigation of Salacia elliptica allowed to the isolation of 20 constituents: two polyols, one xanthone, a mixture of long chain hydrocarbons, one carboxylic acid, one polymer, two steroidal compounds, one aromatic ester and eleven pentacyclic triterpenes. These triterpenes include 3β-stearyloxy-oleanane, 3β-stearyloxy-ursane, one seco-friedelane, and eight compounds of the friedelane serie. The chemical structure and the relative configuration of a new triterpene 1,3-dioxo-16α-hydroxyfriedelane (15) were established through ¹H and 13C NMR including 2D experiments (HMBC, HMQC, COSY and NOESY) and herein reported for the first time.

Chemical constituents of the wood from Zanthoxylum quinduense Tul. (Rutaceae)

Phytochemical investigation of the wood from Zanthoxylum quinduense Tul. allowed the isolation and identification of norchelerythrine, decarine, 6-acetonyldihydrochelerythrine, syringaresinol, evofilin C, p-hydroxybenzaldehyde, vanillic acid, a mixture of β-sitosterol, stigmasterol and campesterol and a mixture of saturated and unsaturated fatty acids, and their esters derivatives. The structures of the isolated compounds were elucidated by spectroscopic techniques and comparison with literature data and the mixture of sterols and fatty acids were identified by GC/MS. The antifungal activity of the ethanolic extract, fractions and pure compounds against Fusarium oxysporum f. sp. lycopersici was determined by bioautography. Evofilin C and nochelerytrine were the only substances that present antifungal activity.

Chemical composition of volatile oils from leaves of Nectandra megapotamica Spreng. (Lauraceae)

The volatile oils from Nectandra megapotamica Spreng. leaves, collected in February and August of 2007 and at 7:00 and 12:00 h (samples A - D), were extracted by hydrodistillation and the chemical composition was analyzed by GC-FID and GC/MS. A total of nineteen compounds were identified with predominance of oxygenated sesquiterpenes, among them, α-bisabolol, was the main constituent (62.3-69.4 %). After chromatographic separation procedures, this compound was purified from crude oil and its structure was confirmed by analysis of NMR data. This paper describes for the first time the composition of the leaves volatile oil from N. megapotamica.