Comparison of three analytical methods for the determination of quinolones in pig muscle samples

This work presents a comparison between three analytical methods developed for the simultaneous determination of eight quinolones regulated by the European Union (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, difloxacin, sarafloxacin, oxolinic acid and flumequine) in pig muscle, using liquid chromatography with fluorescence detection (LC-FD), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The procedures involve an extraction of the quinolones from the tissues, a step for clean-up and preconcentration of the analytes by solid-phase extraction and a subsequent liquid chromatographic analysis. The limits of detection of the methods ranged from 0.1 to 2.1 ng g−1 using LC-FD, from 0.3 to 1.8 using LC-MS and from 0.2 to 0.3 using LC-MS/MS, while inter- and intra-day variability was under 15 % in all cases. Most of those data are notably lower than the maximum residue limits established by the European Union for quinolones in pig tissues. The methods have been applied for the determination of quinolones in six different commercial pig muscle samples purchased in different supermarkets located in the city of Granada (south-east Spain).

Capillary thermal desorption unit for near real-time analysis of VOCs at sub-trace levels. Application to the analysis of environmental air contamination and breath samples

A capillary microtrap thermal desorption module is developed for near real-time analysis of volatile organic compounds (VOCs) at sub-ppbv levels in air samples. The device allows the direct injection of the thermally desorbed VOCs into a chromatographic column. It does not use a second cryotrap to focalize the adsorbed compounds before entering the separation column so reducing the formation of artifacts. The connection of the microtrap to a GC–MS allows the quantitative determination of VOCs in less than 40 min with detection limits of between 5 and 10 pptv (25 °C and 760 mmHg), which correspond to 19–43 ng m−3, using sampling volumes of 775 cm3. The microtrap is applied to the analysis of environmental air contamination in different laboratories of our faculty. The results obtained indicate that most volatile compounds are easily diffused through the air and that they also may contaminate the surrounding areas when the habitual safety precautions (e.g., working under fume hoods) are used during the manipulation of solvents. The application of the microtrap to the analysis of VOCs in breath samples suggest that 2,5-dimethylfuran may be a strong indicator of a person's smoking status

Decay of linkage disequilibrium within genes across HGDP-CEPH human samples: most population isolates do not show increased LD

Background It is well known that the pattern of linkage disequilibrium varies between human populations, with remarkable geographical stratification. Indirect association studies routinely exploit linkage disequilibrium around genes, particularly in isolated populations where it is assumed to be higher. Here, we explore both the amount and the decay of linkage disequilibrium with physical distance along 211 gene regions, most of them related to complex diseases, across 39 HGDP-CEPH population samples, focusing particularly on the populations defined as isolates. Within each gene region and population we use r2 between all possible single nucleotide polymorphism (SNP) pairs as a measure of linkage disequilibrium and focus on the proportion of SNP pairs with r2 greater than 0.8. Results Although the average r2 was found to be significantly different both between and within continental regions, a much higher proportion of r2 variance could be attributed to differences between continental regions (2.8% vs. 0.5%, respectively). Similarly, while the proportion of SNP pairs with r2 > 0.8 was significantly different across continents for all distance classes, it was generally much more homogenous within continents, except in the case of Africa and the Americas. The only isolated populations with consistently higher LD in all distance classes with respect to their continent are the Kalash (Central South Asia) and the Surui (America). Moreover, isolated populations showed only slightly higher proportions of SNP pairs with r2 > 0.8 per gene region than non-isolated populations in the same continent. Thus, the number of SNPs in isolated populations that need to be genotyped may be only slightly less than in non-isolates. Conclusion The 'isolated population' label by itself does not guarantee a greater genotyping efficiency in association studies, and properties other than increased linkage disequilibrium may make these populations interesting in genetic epidemiology.

Three Wavelength Optical Probe for Surface Roughness Measurements of Paper Samples

In the present diploma work optical inspection methods were used to investigate surface roughness of paper samples. A special measurement setup, which includes three laser light sources of three different wavelengths, photodetector and goniometer, was used to measure the reflected laser light properties. The intensity of the light reflected in specular direction was measured versus the laser incidence angle for reference metal sample. The value of roughness was estimated and compared to initially known value of metal sample roughness. Thus, the measurement equipment and method were validated. Then the reflected intensity was measured versus reflection angle at constant incidence angle for the same metal sample and paper samples under investigation. The final values of the surface roughness were obtained from the analysis of the reflected intensity dependence. The results are in good correlation with other research groups.

Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

Ultra-trace amounts of Cu(II) were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone) -2,2-dimethyl-1,3-propanediimine) (SBTD) followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

Bauer-7-en-3beta-yl acetate: a major constituent of unusual samples of Brazilian propolis

The pentacyclic triterpenoid bauer-7-en-3beta-yl acetate was obtained from the chloroform extract of an unusual sample of propolis from southeast Brazil with the yield of 7%. The compound was identified by comparison of IR, MS and NMR analysis with published data.

Removal of chromium (vi) in aqueous environments using cork and heat-treated cork samples from quercus cerris and quercus suber

Chromium (VI) removal and its reduction to chromium (III) from aqueous solution by untreated and heat-treated Quercus cerris and heat-treated Quercus suber black agglomerate cork granules was investigated. Initial screening studies revealed that among the sorbents tested, untreated Q. cerris and Q. suber black agglomerate are the most efficient in the removal of Cr(VI) ions and were selected for adsorption essays. Heat treatment adversely affected chromium adsorption and chromium (VI) reduction in Q. cerris cork. The highest metal uptake was found at pH 3.0 for Q. cerris and pH 2.0 for black agglomerate. The experimental data fitted the Langmuir model and the calculated qmax was 22.98 mg/g in black agglomerate and 21.69 mg/g in untreated Q. cerris cork. The FTIR results indicated that while in black agglomerate, lignin is the sole component responsible for Cr(VI) sorption, and in untreated Q. cerris cork, suberin and polysaccharides also play a significant role on the sorption. The SEM-EDX results imply that chromium has a homogenous distribution within both cork granules. Also, phloemic residues in Q. cerris granules showed higher chromium concentration. The results obtained in this study show that untreated Q. cerris and black agglomerate cork granules can be an effective and economical alternative to more costly materials for the treatment of liquid wastes containing chromium

Community-acquired pneumonia in adult patients with special reference to rapid methods for etiological diagnosis

Aikuispotilaan kotisyntyisen keuhkokuumeen etiologinen diagnostiikka mikrobiologisilla pikamenetelmillä Tausta. Keuhkokuume on vakava sairaus, johon sairastuu Suomessa vuosittain n. 60 000 aikuista. Huolimatta siitä, että taudin hoito on kehittynyt, siihen liittyy yhä merkittävä, 6-15%:n kuolleisuus. Alahengitystieinfektion aiheuttajamikrobien tunnistaminen on myös edelleen haasteellista. Tavoitteet. Tämän työn tavoitteena oli tutkia Turun yliopistollisessa keskussairaalassa hoidettujen aikuispotilaiden keuhkokuumeen etiologiaa sekä selvittää uusien mikrobiologisten pikamenetelmi¬en hyödyllisyyttä taudinaiheuttajan toteamisessa. Aineisto. Osatöiden I ja III aineisto koostui 384 Turun yliopistollisen keskussairaalaan infektio-osastolla hoidetusta keuhkokuumepotilaasta. Osatyössä I tutkittiin keuhkokuumeen aiheuttaja¬mikrobeja käyttämällä perinteisten menetelmien lisäksi antigeeniosoitukseen ja PCR-tekniikkaan perustuvia pikamenetelmiä. Osatyö II käsitti 231 potilaasta koostuvan alaryhmän, jossa tutkittiin potilaiden nielun limanäytteestä rinovirusten ja enterovirusten esiintyvyyttä. Osatyössä III potilailta tutkittiin plasman C-reaktiivisen proteiinin (CRP) pitoisuus ensimmäisten viiden sairaalahoitopäi¬vän aikana. Laajoja tilastotieteellisiä analyysejä käyttämällä selvitettiin CRP:n käyttökelpoisuutta sairauden vaikeusasteen arvioinnissa ja komplikaatioiden kehittymisen ennustamisessa. Osatyössä IV 68 keuhkokuumepotilaan sairaalaan tulovaiheessa otetuista näytteistä määritettiin neutrofiilien pintareseptorien ekspressio. Osatyössä V analysoitiin sisätautien vuodeosastoilla vuosina 1996-2000 keuhkokuumepotilaille tehtyjen keuhkohuuhtelunäytteiden laboratoriotutkimustulokset. Tulokset. Keuhkokuumeen aiheuttaja löytyi 209 potilaalta, aiheuttajamikrobeja löydettiin kaikkiaan 230. Näistä aiheuttajista 135 (58.7%) löydettiin antigeenin osoituksella tai PCR-menetelmillä. Suu¬rin osa, 95 (70.4%), todettiin pelkästään kyseisillä pikamenetelmillä. Respiratorinen virus todettiin antigeeniosoituksella 11.1% keuhkokuumepotilaalla. Eniten respiratorisia viruksia löytyi vakavaa keuhkokuumetta sairastavilta potilailta (20.3%). 231 keuhkokuumepotilaan alaryhmässä todettiin PCR-menetelmällä picornavirus 19 (8.2%) potilaalla. Respiratorinen virus löytyi tässä potilasryh¬mässä kaiken kaikkiaan 47 (20%) potilaalta. Näistä 17:llä (36%) löytyi samanaikaisesti bakteerin aiheuttama infektio. CRP-tasot olivat sairaalaan tulovaiheessa merkitsevästi korkeammat vakavaa keuhkokuumetta (PSI-luokat III-V) sairastavilla potilailla kuin lievää keuhkokuumetta (PSI-luokat I-II) sairastavilla potilailla (p <0.001). Yli 100 mg/l oleva CRP-taso neljän päivän kuluttua sairaa¬laan tulosta ennusti keuhkokuumeen komplikaatiota tai huonoa hoitovastetta. Neutrofiilien komple¬menttireseptorin ekspressio oli pneumokokin aiheuttamaa keuhkokuumetta sairastavilla merkitse¬västi korkeampi kuin influenssan aiheuttamaa keuhkokuumetta sairastavilla. BAL-näytteistä vain yhdessä 71:stä (1.3%) todettiin diagnostinen bakteerikasvu kvantitatiivisessa viljelyssä. Uusilla menetelmilläkin keuhkokuumeen aiheuttaja löytyi vain 9.8% BAL-näytteistä. Päätelmät. Uusilla antigeeniosoitus- ja PCR-menetelmillä keuhkokuumeen etiologia voidaan saada selvitettyä nopeasti. Lisäksi näitä menetelmiä käyttämällä taudin aiheuttajamikrobi löytyi huomattavasti suuremmalta osalta potilaista kuin pelkästään tavanomaisia menetelmiä käyttämällä. Pikamenetelmien hyödyllisyys vaihteli taudin vaikeusasteen mukaan. Respiratorinen virus löytyi huomattavan usein keuhkokuumetta sairastavilta potilailta, ja näiden potilaiden taudinkuva oli usein vaikea. Tulovaiheen korkeaa CRP-tasoa voidaan käyttää lisäkeinona arvioitaessa keuhkokuumeen vaikeutta. CRP on erityisen hyödyllinen arvioitaessa hoitovastetta ja riskiä komplikaatioiden ke¬hittymiseen. Neutrofiilien komplementtireseptorin ekspression tutkiminen näyttää lupaavalta pi¬kamenetelmältä erottamaan bakteerien ja virusten aiheuttamat taudit toisistaan. Antimikrobihoitoa saavilla potilailla BAL-tutkimuksen löydökset olivat vähäiset ja vaikuttivat hoitoon vain harvoin.

Determination of chemical elements in africanized Apis mellifera (Hymenoptera: Apidae) honey samples from the State of Piauí, Brazil

Honey is a food used since the most remote times, appreciated for its characteristic flavor, considerable nutritional value and medicinal properties; however, little information exists about the presence of chemical elements in it. The objectives of this work were to determine the chemical elements present in 38 honey samples, collected directly from beekeepers from the State of Piauí, Brazil and to verify whether they presented any contamination. The chemical elements were determined by means of Total Reflection X-ray Fluorescence. The means of three replicates were: K (109.671 ± 17.487), Ca (14.471 ± 3.8797), Ti (0.112 ± 0.07), Cr (0.196 ± 0.11), Mn (0.493 ± 0.103), Fe (1.722 ± 0.446), Co (0.038), Ni (0.728 ± 0.706), Cu (0.179 ± 0.0471), Zn (0.967 ± 0.653), Se (not detected), Br (not detected), Rb (0.371 ± 0.097), Sr (0.145 ± 0.45), Ba (11.681), Hg (not detected), and Pb (0.863) µg g-1.

Ewing sarcoma of the rib: respiratory tract infection as initial symptoms in a 14-year-old boy. Functional medical imaging findings

Ewing sarcoma or primitive neuroectodermal tumor (PNET) of bone is the second most common pediatric malignant bone tumor. The median age at diagnosis is 15 years and there is a male predilection of 1.5/1. The authors present the case of a 14-year-old boy with Ewing sarcoma situated on the left ninth rib which was being investigated for respiratory tract infection. Pleurisy is the most common misdiagnosis. Our case illustrates the importance of recognizing exceptional features when interpreting FDG PET or scintigraphy to prevent the misinterpretation of metastases as other etiologies, such as infection.

Physicochemical composition of Apis mellifera honey samples from São Paulo State, Brazil

This research, developed with Apis mellifera honey samples from producers of São Paulo State, Brazil, has the objective of verifying how eucalyptus, wild flower, and orange honey samples would be clustered, based on physicochemical characteristics. All the orange honey samples and some wild flower ones formed distinct groups, thus confirming that the floral source interferes with honey characteristics. Eucalyptus and some of the wild flower honey samples were clustered together because of the great floral source variation in the latter ones. The characteristics that influence sample clustering are acidity and electric conductivity on the X axis, and total sugars and pH on the Y axis.

Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU), copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4) of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

Characterizing Propionibacterium freudenreichii ssp. shermanii JS and Lactobacillus rhamnosus LC705 as a new probiotic combination: basic properties of JS and pilot in vivo assessment of the combination

Characterizing Propionibacterium freudenreichii ssp. shermanii JS and Lactobacillus rhamnosus LC705 as a new probiotic combination: basic properties of JS and pilot in vivo assessment of the combination Each candidate probiotic strain has to have the documentation for the proper identification with current molecular tools, for the biological properties, for the safety aspects and for the health benefits in human trials if the intention is to apply the strain as health promoting culture in the commercial applications. No generalization based on species properties of an existing probiotic are valid for any novel strain, as strain specific differences appear e.g. in the resistance to GI tract conditions and in health promoting benefits (Madsen, 2006). The strain evaluation based on individual strain specific probiotic characteristics is therefore the first key action for the selection of the new probiotic candidate. The ultimate goal in the selection of the probiotic strain is to provide adequate amounts of active, living cells for the application and to guarantee that the cells are physiologically strong enough to survive and be biologically active in the adverse environmental conditions in the product and in GI tract of the host. The in vivo intervention studies are expensive and time consuming; therefore it is not rational to test all the possible candidates in vivo. Thus, the proper in vitro studies are helping to eliminate strains which are unlikely to perform well in vivo. The aims of this study were to characterize the strains of Propionibacterium freudenreichii ssp. shermanii JS and Lactobacillus rhamnosus LC705, both used for decades as cheese starter cultures, for their technological and possible probiotic functionality applied in a combined culture. The in vitro studies of Propionibacterium freudenreichii ssp. shermanii JS focused on the monitoring of the viability rates during the acid and bile treatments and on the safety aspects such as antibiotic susceptibility and adhesion. The studies with the combination of the strains JS and LC705 administered in fruit juices monitored the survival of the strains JS and LC705 during the GI transit and their effect on gut wellbeing properties measured as relief of constipation. In addition, safety parameters such as side effects and some peripheral immune parameters were assessed. Separately, the combination of P. freudenreichii ssp. shermanii JS and Lactobacillus rhamnosus LC705 was evaluated from the technological point of view as a bioprotective culture in fermented foods and wheat bread applications. In this study, the role ofP. freudenreichii ssp. shermanii JS as a candidate probiotic culture alone and in a combination with L. rhamnosus LC705 was demonstrated. Both strains were transiently recovered in high numbers in fecal samples of healthy adults during the consumption period. The good survival through the GI transit was proven for both strains with a recovery rate from 70 to 80% for the JS strain and from 40 to 60% for the LC705 strain from the daily dose of 10 log10 CFU. The good survival was shown from the consumption of fruit juices which do not provide similar matrix protection for the cells as milk based products. The strain JS did not pose

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH) in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(a)pyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.