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61.
Jani Koponen Hannu Kiviranta 《International journal of environmental analytical chemistry》2013,93(13):1268-1285
ABSTRACTIn this paper, we present the results of an analytical method that has been recently developed, validated and successfully applied in a biomonitoring approach. In the environmental pollutant studies it is desirable that the analytical method can determine multiple classes of compounds from a single, small volume sample. The presented analytical method with a simple sample pre-treatment allows the quantitation of 13 perfluoroalkyl acids (PFAAs), 6 parabens and cotinine (used as nicotine biomarker) from a single, small volume of 100 µL serum sample by liquid chromatography-triple quadrupole mass spectrometer (LC-MS/MS). The limits of quantitation (LOQ) for PFAAs, parabens and cotinine were 0.10–0.50, 0.20–0.80 and 0.10 ng/mL, respectively. Besides sensitivity the method has excellent trueness/accuracy and repeatability. The trueness of the method for the determination of PFAAs ranged from 95% to 106% and the repeatability (as RSD %) from 0.6% to 5.6%. The accuracy and RSD for parabens were 73–120% and 1.3–9.7%, respectively, and 100–106% and 1.3–3.5 % for cotinine. Biomonitoring data reveals the presence of several PFAAs and parabens in serum samples of Finnish population. The total concentrations for PFAAs and parabens were from 2.0 to 33 ng/mL and from <LOQ to 1100 ng/mL, respectively. Nearly all non-smokers had the serum cotinine concentration below 1.0 ng/mL, which can be suggested as the cut point for cotinine concentration to identify smoking. 相似文献
62.
Vera Homem Arminda Alves 《International journal of environmental analytical chemistry》2013,93(14-15):1063-1084
The adsorption of the antibiotic amoxicillin at low concentration levels (µg?L?1 order) from aqueous solution on almond shell ashes has been investigated, either by kinetic or equilibrium assays. The effect of the adsorbent amount, initial concentration of the antibiotic, particle diameter (dp) and temperature were considered to evaluate the adsorption capacity of the adsorbent. The results showed that amoxicillin sorption is dependent on these four factors. The adsorption process was relatively fast and equilibrium was established in about 12 hours. The optimum parameters for an initial concentration of 450?µg?L?1 were 50?mg of adsorbent, 303?K and dp?<?600?µm. A comparison of kinetic models showed that pseudo-second order kinetics provides the best correlation of the experimental data. Isotherm data adjusted better to Langmuir equation, with an adsorption capacity of 2.5?±?0.1?mg?g?1 at 303?K. The desorption process was also evaluated (maximum efficiency of 5%). Thermodynamic parameters were calculated and the negative value of ΔH0 and ΔG0 showed that adsorption was exothermic and a spontaneous process. 相似文献
63.
Vera Homem Raquel Sousa José Luís Moreira Lúcia Santos 《International journal of environmental analytical chemistry》2013,93(2):166-189
A new method for the simultaneous determination of 12 volatile organic compounds (trans-1,2-dichloroethene, 1,1,1-trichloroethane, benzene, 1,2-dichloroethane, trichloroethene, toluene, 1,1,2-trichloroethane, tetrachloroethene, ethylbenzene, m-, p-, o-xylene) in water samples by headspace solid phase microextraction (HS–SPME)–gas chromatography mass spectrometry (GC–MS) was described, using a 100?µm PDMS (polydimethylsiloxane) coated fibre. The response surface methodology was used to optimise the effect of the extraction time and temperature, as well as the influence of the salt addition in the extraction process. Optimal conditions were extraction time and temperature of 30?min and ?20°C, respectively, and NaCl concentration of 4?mol?L?1. The detection limits were in the range of 1.1?×?10?3–2.3?µg?L?1 for the 12 volatile organic compounds (VOCs). Global uncertainties were in the range of 4–68%, when concentrations decrease from 250?µg?L?1 down to the limits of quantification. The method proved adequate to detect VOCs in six river samples. 相似文献
64.
Two new synthetic methodologies for 2,3-diarylacridin-9(10H)-ones were developed. The first one involves the Heck reaction of (E)-3-iodo-2-styrylquinolin-4(1H)-ones with styrenes, leading to (E,E)-2,3-distyrylquinolin-4(1H)-ones, which when heated at high temperatures cyclize in two different ways. Electrocyclization and further in situ oxidation leads to 2,3-diarylacridin-9(10H)-ones, while tautomerization, cyclization by nucleophilic addition and further in situ oxidation produces (E)-2-aryl-4-styrylfuro[3,2-c]quinolines as the main compound. The second method gives only 2,3-diaryl-10-methylacridin-9(10H)-ones and involves the Heck reaction of (E)-3-iodo-1-methyl-2-styrylquinolin-4(1H)-ones and styrenes, leading to (E,E)-1-methyl-2,3-distyrylquinolin-4(1H)-ones, which when heated at high temperatures cyclize through electrocyclization and oxidation processes affording the expected compounds. The structures of all new compounds were established by extensive NMR studies. 相似文献
65.
Roseane Pagliaro Avegliano Vera Akiko Maihara 《Journal of Radioanalytical and Nuclear Chemistry》2014,299(1):781-785
Total Diet Studies (TDS) have been carried out to estimate dietary intakes of the essential and toxic elements for a large-scale population over a specific period of time. In this study, the TDS was based on the evaluation of food representing a Market Basket (MB), which reflected the dietary habits of the São Paulo State population, corresponding to 72 % of the average food consumption for the state of São Paulo. In the present Total Diet Study, magnesium and manganese concentrations were determined in 30 of the most consumed food groups of a MB of São Paulo State, Brazil. Instrumental Neutron Activation Analysis (INAA) has been successfully used on a regularly basis in several areas of nutrition and foodstuffs. Element concentrations were determined by INAA in freeze-dried samples and ranged in mg kg?1. Mg 41.4 (fats)–5287 (coffee) and Mn 0.12 (prime grade beef)–32.9 (coffee). The average daily Mg and Mn intake was calculated by multiplying the concentration of each element in each table-ready food group by the respective weight (g day?1) of the food group in the MB and adding the products from all food groups. The results of daily dietary intakes in this study were: Mg 174.8 and Mn 1.34 mg day?1. Theses values were lower than the adequate intake (AI) proposed by the Food and Nutrition Board of the Institute of Medicine (USA National Academy) for adults. The low levels of Mg and Mn intakes presented in this TDS are probably due to the fact that MB of this study represented only 72 % of the weight of the most consumed household foods of São Paulo State. 相似文献
66.
Marildes Josefina Lemos Neto Elizabeth de Souza Nascimento Vera Akiko Maihara Paulo Sergio C. Silva Mariza Landgraf 《Journal of Radioanalytical and Nuclear Chemistry》2014,300(2):573-579
Three CRMs of different matrix composition were analysed, representing an environmental matrix sample (BCR–320R Channel Sediment), a botanical matrix sample (SRM 1547 Peach Leaves) and a zoological matrix sample (SRM 1566b Oyster Tissue). The element mass fractions were obtained using the KayWin program. Analytical measurement uncertainty was determined by two approaches: (1) the routine procedure applying combination of the overall uncertainty u(m) = 3.5 % and statistical uncertainty of the peak area determination and (2) the procedure applying the dedicated ERON program for calculating uncertainty. Performance of altogether 31 certified values was tested by means of calculating E n numbers. For the remaining 52 non-certified values, comparison between uncertainties obtained by the two approaches was made. When using the first approach, the E n number showed satisfactory performance in 28 cases; by using the second approach, the E n number showed satisfactory performance in 27 cases. None of the unsatisfactory performances (E n > 1) appeared to be of systematic nature. The uncertainties obtained by applying the two approaches revealed a big extent of consistency. As the present nuclear database lacks lot of data that serve as input to the ERON program, in particular uncertainties of Q 0 factors, estimates need to be introduced for the missing values, emphasising the urgent need to upgrade the database with missing data. 相似文献
67.
Johanna Rajasärkkä Jani Koponen Riikka Airaksinen Hannu Kiviranta Marko Virta 《Analytical and bioanalytical chemistry》2014,406(23):5695-5702
Bioluminescent Saccharomyces cerevisiae yeast-based bioreporters were used to monitor bisphenol A and other estrogenic chemicals in thermal paper samples collected mainly from Finland on two occasions in 2010/2011, and 2013. The bisphenol A-targeted (BPA-R) and the human oestrogen receptor (hERα) bioreporters were applied to analyse both non-treated and extracted paper samples. Bisphenol A was readily bioavailable to the yeast bioreporters on the non-treated paper samples without any pre-treatment. Detected concentrations ranged from a detection limit of 9–142 μg/g to over 20 mg/g of bisphenol A equivalents in the thermal papers. Low bisphenol A like activities were detected in many samples, and were considered to be caused by residual bisphenol A or other types of bisphenols, such as bisphenol S. Most of the thermal paper samples were toxic to the yeast bioreporters. The toxicity did not, however, depend on the bisphenol A concentration of the samples. The yeast bioreporters were demonstrated to be a robust and cost-efficient method to monitor thermal paper samples for their bisphenol A content and estrogenicity. Thermal paper was considered as a potential BPA source for both human exposure and environmental emission. 相似文献
68.
Fbio Bernardo Providencia Gonzlez-Hernndez Nuno Ratola Vernica Pino Arminda Alves Vera Homem 《Molecules (Basel, Switzerland)》2021,26(11)
Volatile methylsiloxanes (VMSs) constitute a group of compounds used in a great variety of products, particularly personal care products. Due to their massive use, they are continually discharged into wastewater treatment plants and are increasingly being detected in wastewater and in the environment at low concentrations. The aim of this work was to develop and validate a fast and reliable methodology to screen seven VMSs in water samples, by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The influence of several factors affecting the extraction efficiency was investigated using a design of experiments approach. The main factors were selected (fiber type, sample volume, ionic strength, extraction and desorption time, extraction and desorption temperature) and optimized, employing a central composite design. The optimal conditions were: 65 µm PDMS/Divinylbenzene fiber, 10 mL sample, 19.5% NaCl, 39 min extraction time, 10 min desorption time, and 33 °C and 240 °C as extraction and desorption temperature, respectively. The methodology was successfully validated, showing low detection limits (up to 24 ng/L), good precision (relative standard deviations below 15%), and accuracy ranging from 62% to 104% in wastewater, tap, and river water samples. 相似文献
69.
We present phase diagrams for a polarized Fermi gas in an optical lattice as a function of temperature, polarization, and lattice filling factor. We consider the Fulde-Ferrel-Larkin-Ovchinnikov (FFLO), Sarma or breached pair, and BCS phases, and the normal state and phase separation. We show that the FFLO phase appears in a considerable portion of the phase diagram. The diagrams have two critical points of different nature. We show how various phases leave clear signatures to momentum distributions of the atoms which can be observed after time of flight expansion. 相似文献
70.
Krasnov Victor P. Zarubaev Vladimir V. Gruzdev Dmitry А. Vozdvizhenskaya Olga А. Vakarov Sergey А. Musiyak Vera V. Chulakov Evgeny N. Volobueva Alexandrina S. Sinegubova Ekaterina O. Ezhikova Marina А. Kodess Mikhail I. Levit Galina L. Charushin Valery N. 《Chemistry of Heterocyclic Compounds》2021,57(4):498-504
Chemistry of Heterocyclic Compounds - A number of novel amides were synthesized by coupling of 6-[(9H-purin-6-yl)amino]hexanoic acid to heterocyclic amines. The antiviral activity of the obtained... 相似文献