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Showing papers in "International Journal of Analytical Chemistry in 2012"


Journal ArticleDOI
TL;DR: The present review has described the development of Electrospray Ionization mass spectrometry (ESI-MS) during the last 25 years in the study of various properties of different types of biological molecules.
Abstract: The Electrospray Ionization (ESI) is a soft ionization technique extensively used for production of gas phase ions (without fragmentation) of thermally labile large supramolecules. In the present review we have described the development of Electrospray Ionization mass spectrometry (ESI-MS) during the last 25 years in the study of various properties of different types of biological molecules. There have been extensive studies on the mechanism of formation of charged gaseous species by the ESI. Several groups have investigated the origin and implications of the multiple charge states of proteins observed in the ESI-mass spectra of the proteins. The charged analytes produced by ESI can be fragmented by activating them in the gas-phase, and thus tandem mass spectrometry has been developed, which provides very important insights on the structural properties of the molecule. The review will highlight recent developments and emerging directions in this fascinating area of research.

519 citations


Journal ArticleDOI
TL;DR: In this study a range of flavonoid standards are investigated by chip-based negative ion nanospray mass spectrometry and it was found that the different classes of Flavonoid studied have a combination of distinct neutral losses from the precursor ion [M-H]− along with characteristic low-mass ions.
Abstract: Flavonoids are one of the most important classes of natural products having a wide variety of biological activities. There is wide interest in a range of medical and dietary applications, and having a rapid, reliable method for structural elucidation is essential. In this study a range of flavonoid standards are investigated by chip-based negative ion nanospray mass spectrometry. It was found that the different classes of flavonoid studied have a combination of distinct neutral losses from the precursor ion [M-H]− along with characteristic low-mass ions. By looking only for this distinct pattern of product ions, it is possible to determine the class of flavonoid directly. This methodology is tested here by the analysis of a green tea extract, where the expected flavonoids were readily identified, along with quercetin, which is shown to be present at only about 2% of the most intense ion in the spectrum.

95 citations


Journal ArticleDOI
TL;DR: The proposed method was validated to be simple and reliable and can be a tool for quality control of bamboo leaf extract or its commercial products.
Abstract: A strategy for analyzing flavone C-glucosides in the leaves of different species of bamboo was developed. Firstly, the flavone C-glycosides were extracted from the bamboo leaves (51 species in 17 genera) with methanol and chromatographed on silica gel 60 plates in automatic developing chamber (ADC2), and a qualitative survey using simple derivatization steps with the NP reagent was carried out. The flavone C-glycosides were found in 40 of 51 species of bamboo examined. Secondly, an HPLC method with photodiode array and multiple wavelength detector was optimized and validated for the simultaneous determination of flavone C-glycosides, including isoorientin, isovitexin, orientin, and vitexin in the leaves of three species of bamboo and the flavone C-glycosides were confirmed by LC/MS. The optimized HPLC method proved to be linear in the concentration range tested (0.2–100 μg/mL, ), precise (%), and accurate (88–106%). The concentration ranges of isoorientin, isovitexin, orientin, and vitexin in three bamboo leaves samples were 1.00–2.78, 0–0.31, 0–0.07, and 0.20–0.68 mg/g, respectively. The proposed method was validated to be simple and reliable and can be a tool for quality control of bamboo leaf extract or its commercial products.

41 citations


Journal ArticleDOI
Baosheng Liu1, Chao Yang1, Xiaona Yan1, Jing Wang1, Yun-Kai Lv1 
TL;DR: The interaction between Avelox and bovine serum albumin (BSA) was investigated at different temperatures by fluorescence spectroscopy and clearly revealed that the microenvironment of amino acid residues and the conformation of BSA were changed during the binding reaction.
Abstract: The interaction between Avelox and bovine serum albumin (BSA) was investigated at different temperatures by fluorescence spectroscopy. Results showed that Avelox could quench the intrinsic fluorescence of BSA strongly, and the quenching mechanism was a static quenching process with Forester spectroscopy energy transfer. The electrostatic force played an important role on the conjugation reaction between BSA and Avelox. The order of magnitude of binding constants () was 104, and the number of binding site () in the binary system was approximately equal to 1. The binding distance () was less than 3 nm and the primary binding site for Avelox was located in subdomain IIA of BSA. Synchronous fluorescence spectra clearly revealed that the microenvironment of amino acid residues and the conformation of BSA were changed during the binding reaction. In addition, the effect of some antibiotics on the binding constant of Avelox with BSA was also studied.

24 citations


Journal ArticleDOI
TL;DR: A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals and is successfully employed in the analysis of various biological, water, and alloy samples for the determined iron and cobalt content.
Abstract: Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH) reacts with iron(II) and cobalt(II) to form reddish-brown and yellow-coloured [Fe(II)-HNAHBH] and [Co(II)-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II)-HNAHBH], Beer’s law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II)-HNAHBH] complex obeys Beer’s law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content.

19 citations


Journal ArticleDOI
TL;DR: It was showed that the presence of gum increases the stability of the films in acidic medium and the performance of the modified electrode of PANI-PA/CG was evaluated in electro analytical determination of dopamine (DA).
Abstract: We take advantage of polyelectrolyte feature exhibited by natural cashew gum (Anacardium occidentale L.) (CG), found in northeast Brazil, to employ it in the formation of electroactive nanocomposites prepared by layer-by-layer (LbL) technique. We used polyaniline unmodified (PANI) or modified with phosphonic acid (PA), PANI-PA as cationic polyelectrolyte. On the other hand, the CG or polyvinyl sulfonic (PVS) acids were used as anionic polyelectrolytes. The films were prepared with PANI or PANI-PA intercalated with CG or with PVS alternately resulting in four films with different sequences: PANI/CG PANI-PA/CG, PANI/PVS and PANI-PA/PVS, respectively. Analysis by cyclic voltammetry (CV) of the films showed that the presence of gum increases the stability of the films in acidic medium. The performance of the modified electrode of PANI-PA/CG was evaluated in electro analytical determination of dopamine (DA). The tests showed great sensitivity of the film for this analyte that was detected at 10−5 mol L−1.

16 citations


Journal ArticleDOI
TL;DR: The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples and will present a wide application in the future.
Abstract: An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF6] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L−1 and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future.

16 citations


Journal ArticleDOI
TL;DR: The chemical composition of essential oil described in this paper differs from that described in the literature for L. sidoides found in its native environment, where the major constituents are thymol and carvacrol.
Abstract: Several studies involving the family Verbenaceae, occurring in the Brazilian Cerrado, have emphasized the popular use of many aromatic species. We highlight the use of Lippia sidoides Cham., known as “alecrim pimenta,” native to northeastern Brazil and northern Minas Gerais. Leaves of this species were collected in antropized Brazilian Cerrado area, in Hidrolândia, Goias, and their essential oils were extracted by hydrodistillation in a Clevenger-type apparatus and thereafter analyzed GC/MS. Among the compounds identified in this study were the most abundant oxygenated monoterpenes, followed by sesquiterpenes hydrocarbons. The oxygenated monoterpene 1,8-cineole was the major constituent followed by isoborneol and bornyl acetate. The chemical composition of essential oil described in this paper differs from that described in the literature for L. sidoides found in its native environment, where the major constituents are thymol and carvacrol.

15 citations


Journal ArticleDOI
TL;DR: Tin presence at low-concentration range was successfully determined and it was shown that tenth times less concentrations of Sn were present in protected cans than in nonprotected or partially protected tinplate.
Abstract: Tin content in samples of canned fruits and vegetables was determined by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-OES), and it was compared with results obtained by standard method of flame atomic absorption spectrometry (AAS). Selected tin emission lines intensity was measured in prepared samples after addition of tartaric acid and followed by hydride generation with sodium borohydride solution. The most favorable line at 189.991 nm showed the best detection limit (1.9 μg L−1) and limit of quantification (6.4 μg kg−1). Good linearity and sensitivity were established from time resolved analysis and calibration tests. Analytical accuracy of 98–102% was obtained by recovery study of spiked samples. Method of standard addition was applied for tin determination in samples from fully protected tinplate. Tin presence at low-concentration range was successfully determined. It was shown that tenth times less concentrations of Sn were present in protected cans than in nonprotected or partially protected tinplate.

15 citations


Journal ArticleDOI
TL;DR: A competitive CZE method for quality control analysis of multivitamin preparations and veterinary products containing B-group vitamins was developed and the proposed method was validated demonstrating the good reliability of this method.
Abstract: A competitive CZE method for quality control analysis of multivitamin preparations and veterinary products containing B-group vitamins was developed. Vitamins of interest are thiamine hydrochloride (B 1), thiamine monophosphate chloride (B 1a), riboflavine (B 2), riboflavine-5′monophosphate (B 2a), nicotinamide (B 3), d-pantothenic acid calcium salt (B 5), pyridoxine hydrochloride (B 6), folic acid (B 9), and 4-aminobenzoic acid (B 10). These analytes were separated optimizing the experimental conditions in 20 mM tetraborate buffer p H = 9 . 2 as a BGE (background electrolyte), on a Beckman P/ACE System MDQ instrument, using uncoated fused silica capillary. The effective capillary length was of 49.5 cm, I . D . = 5 0 μm, the applied voltage 20 kV and the temperature 25 ∘C. Detection was performed by a diode array detector at 214 nm for all vitamins except B 5 (190 nm) and B 2a (260 nm). Separation time was about 9 min. After experimental conditions optimization, the proposed method was validated. Precision of migration time and corrected peak area, linearity range, LOD and LOQ, accuracy (recovery), robustness, and ruggedness were evaluated for each analyte demonstrating the good reliability of the method. Analyses of the pharmaceutical real samples were performed and confirmed the versatility of this method.

15 citations


Journal ArticleDOI
TL;DR: The field study showed performance comparable to that in laboratory and yielded first measurements of TMSOH, ranging from 1.02 to 27.30 μg/m3, in the semiconductor industry, and suggested future development of real-time monitoring techniques for TMSoh and other siloxanes for better maintenance and control of scanner lens in semiconductor wafer manufacturing.
Abstract: Trimethylsilanol (TMSOH) can cause damage to surfaces of scanner lenses in the semiconductor industry, and there is a critical need to measure and control airborne TMSOH concentrations. This study develops a thermal desorption (TD)-gas chromatography (GC)-mass spectrometry (MS) method for measuring trace-level TMSOH in occupational indoor air. Laboratory method optimization obtained best performance when using dual-bed tube configuration (100 mg of Tenax TA followed by 100 mg of Carboxen 569), n-decane as a solvent, and a TD temperature of 300°C. The optimized method demonstrated high recovery (87%), satisfactory precision (<15% for spiked amounts exceeding 1 ng), good linearity (R2=0.9999), a wide dynamic mass range (up to 500 ng), low method detection limit (2.8 ng m−3 for a 20-L sample), and negligible losses for 3-4-day storage. The field study showed performance comparable to that in laboratory and yielded first measurements of TMSOH, ranging from 1.02 to 27.30 μg/m3, in the semiconductor industry. We suggested future development of real-time monitoring techniques for TMSOH and other siloxanes for better maintenance and control of scanner lens in semiconductor wafer manufacturing.

Journal ArticleDOI
TL;DR: The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.
Abstract: A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250 mm × 4.6 mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333 nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 and N-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15 M SDS-6% (v/v)-pentanol-0.01 M NaH2PO4 buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (𝑟g0.999), limit of detection (5 and 18 ng mL−1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50 ng mL−1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

Journal ArticleDOI
TL;DR: This work is the first to report that the antimicrobial peptide and NiTsPc LbL film exhibits electroanalytical activity to DA oxidation, a fundamental aspect for the development of electrochemical sensors with potential applications in the biomedical and pharmaceutical industries.
Abstract: The antimicrobial peptide dermaseptin 01 (DS 01), from the skin secretion of Phyllomedusa hypochondrialis frogs, was immobilized in nanostructured layered films in conjunction with nickel tetrasulfonated phthalocyanines (NiTsPc), widely used in electronic devices, using layer-by-layer technique. The films were used as a biosensor to detect the presence of dopamine (DA), a neurotransmitter associated with diseases such as Alzheimer's and Parkinson's, with detection limits in the order of 10−6 mol L−1. The use of DS 01 in LbL film generated selectivity in the detection of DA despite the presence of ascorbic acid found in biological fluids. This work is the first to report that the antimicrobial peptide and NiTsPc LbL film exhibits electroanalytical activity to DA oxidation. The selectivity in the detection of DA is a fundamental aspect for the development of electrochemical sensors with potential applications in the biomedical and pharmaceutical industries.

Journal ArticleDOI
TL;DR: A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood and proved to be specific and linear over the range.
Abstract: A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (; 1.8 μm), at 35°C. The mobile phase consisted of acetonitrile (70%) and ammonium formate 5 mM (30%). Total run time was 1.5 min operating at isocratic mode with a flow rate of 0.3 mL/min. Mass spectrometry detection was performed by positive mode electrospray, on the ammonium adducts with two transitions for each analyte and one for the IS (d3-digoxin). The method proved to be specific and linear over the range (0.3–10) ng/mL. This technique also showed high sensitivity with a 0.09 ng/mL LOD and a 0.28 ng/mL LOQ, for both substances. Percentage recovery ranged from 83 to 100% for digoxin and from 62 to 94% for metildigoxin. The intra- and interday precision CV were ≤10%.

Journal ArticleDOI
TL;DR: The designed biosensor possesses good stability and reproducibility and achieves 95% of the steady-state current in less than five seconds.
Abstract: We investigated the electrochemical behavior of hemoglobin by glassy carbon electrode modified with Mn2O3-Ag nanofibers. The Mn2O3-Ag nanofibers were used as facilitator electron transfer between Hb and glassy-carbon-modified electrode. The Mn2O3-Ag nanofibers are studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The hemoglobin showed a quasireversible electrochemical redox behavior with a formal potential of −49 mV (versus Ag/AgCl) in 0.1 M potassium phosphate buffer solution at pH 7.0. The designed biosensor possesses good stability and reproducibility and achieves 95% of the steady-state current in less than five seconds.

Journal ArticleDOI
TL;DR: The biorecognition method is reproducible and shows high specificity and good accuracy, and the capture assay platform shows a promising approach to patterning dendrimers for nanotechnology applications.
Abstract: Immunoimaging scanning probe microscopy was utilized for the low-level detection and quantification of biotinylated G4 poly(amidoamine) PAMAM dendrimers. Results were compared to those of high-performance liquid chromatography (HPLC) and found to provide a vastly improved analytical method for the low-level detection of dendrimers, improving the limit of detection by a factor of 1000 (LOD=2.5×10−13 moles). The biorecognition method is reproducible and shows high specificity and good accuracy. In addition, the capture assay platform shows a promising approach to patterning dendrimers for nanotechnology applications.

Journal ArticleDOI
TL;DR: The results suggest that CSD increases the stability of the dried extract of G. ulmifolia, with and without added colloidal silicon dioxide.
Abstract: We report the results of a preliminary estimation of the stability of the dried extract from bark of Guazuma ulmifolia Lam. (“Mutamba”), with and without added colloidal silicon dioxide (CSD). The physical and chemical properties and the compatibility of CSD in the extract were evaluated for 21 days of storage under stress conditions of temperature (45 ± 2°C) and humidity (75 ± 5%). Thermogravimetry (TG) was supplemented using selective high-performance liquid chromatography (HPLC) for determination of stability of the characteristic constituents (chemical markers), namely, procyanidin B2 (PB2) and epicatechin (EP). The results showed that PB2 is an appropriate compound to be used as a chemical marker in the quality control of dried extracts of G. ulmifolia. The stress study showed that there was no significant difference between the two formulations. However, considering the TG data and the high temperatures involved, the results suggest that CSD increases the stability of the dried extract of G. ulmifolia.

Journal ArticleDOI
TL;DR: To evaluate samples of industrial and alembic sugar cane spirits from Cape Verde and Ceará, Brazil using principal component analysis, volatile organic compounds, copper; and sulfates were analyzed.
Abstract: Sugar cane spirits are some of the most popular alcoholic beverages consumed in Cape Verde. The sugar cane spirit industry in Cape Verde is based mainly on archaic practices that operate without supervision and without efficient control of the production process. The objective of this work was to evaluate samples of industrial and alembic sugar cane spirits from Cape Verde and Ceara, Brazil using principal component analysis. Thirty-two samples of spirits were analyzed, twenty from regions of the islands of Cape Verde and twelve from Ceara, Brazil. Of the samples obtained from Ceara, Brazil seven are alembic and five are industrial spirits. The components analyzed in these studies included the following: volatile organic compounds (n-propanol, isobutanol, isoamylic, higher alcohols, alcoholic grade, acetaldehyde, acetic acid, acetate); copper; and sulfates.

Journal ArticleDOI
TL;DR: Hyphenated techniques of gas chromatography coupled to mass spectrometer were used to determine fatty acids in eleven species of seaweeds from Fernando de Noronha archipelago finding no specificity in the presence of a particular set of fatty acids and the studied species indicating that they are not useful as taxonomic indicators.
Abstract: Hyphenated techniques of gas chromatography coupled to mass spectrometer were used to determine fatty acids in eleven species of seaweeds from Fernando de Noronha archipelago. The main compounds detected in all studied species were the alcohol phytol and the fatty acids 14 : 0; 15 : 0; 16 : 0; 18 : 0; 18 : 1 n9; 18 : 2 Δ9,12; 20 : 4; 20 : 5. These fatty acids are commonly found in seaweeds present in warm regions. Thus, we found no specificity in the presence of a particular set of fatty acids and the studied species indicating that they are not useful as taxonomic indicators. However, they could be used in a comparative study with algae found in polluted area because many of the studied seaweeds are widespread and Fernando de Noronha has low human influence.

Journal ArticleDOI
TL;DR: High-resolution paper spray spectra were obtained for both organic and biological samples to demonstrate the benefit of linking the technique with a high-resolution mass analyzer.
Abstract: Paper Spray Ionization is an atmospheric pressure ionization technique that utilizes an offline electro-osmotic flow to generate ions off a paper medium. This technique can be performed on a Bruker SolariX Fourier transform ion cyclotron resonance mass spectrometer by modifying the existing nanospray source. High-resolution paper spray spectra were obtained for both organic and biological samples to demonstrate the benefit of linking the technique with a high-resolution mass analyzer. Error values in the range 0.23 to 2.14 ppm were obtained for calf lung surfactant extract with broadband mass resolving power (m/Δm50%) above 60,000 utilizing an external calibration standard.

Journal ArticleDOI
TL;DR: SRTXRF was used to determine As, Ba, Br, Ca, Co, Cr, Cs, Cu, Dy, Fe, K, Mn, Mo, Ni, Pb, Rb, Sr, Ti, V, and Zn in eleven seaweed species commonly found in Fernando de Noronha to provide baseline information about the absorption and accumulation of these elements by macroalgae in the area.
Abstract: SRTXRF was used to determine As, Ba, Br, Ca, Co, Cr, Cs, Cu, Dy, Fe, K, Mn, Mo, Ni, Pb, Rb, Sr, Ti, V, and Zn in eleven seaweed species commonly found in Fernando de Noronha: Caulerpa verticillata (J. Agardh) (Chlorophyta), Asparagopsis taxiformis (Delile), Dictyurus occidentalis (J. Agardh), Galaxaura rugosa (J. Ellis & Solander) J. V. Lamouroux, G. obtusata (J. Ellis & Solander) J. V. Lamouroux, G. marginata (J. Ellis & Solander) J. V. Lamouroux (Rhodophyta), Dictyota cervicornis (Kutzing), Dictyopteris justii (J. V. Lamouroux), Dictyopteris plagiogramma (Montagne) Vickers, Padina gymnospora (Kutzing) Sonder, and a Sargassum sp. (Phaeophyta). Data obtained were compared to those from the analysis of other parts of the world seaweeds using different analytical techniques and were found to be in general agreement in terms of major and minor elemental components. Results provide baseline information about the absorption and accumulation of these elements by macroalgae in the area.

Journal ArticleDOI
TL;DR: The immunoaffinity concentration of glycyrrhizin was determined by immunoAffinity column conjugated with antiginsenoside Rb1 and Rg1 MAbs resulting in the glycynRHizin-knockout extract, which was determinedBy the synergic effect with glycyRrhiz in on NO production using the cell line.
Abstract: Matrix-assisted laser desorption/ionization (MALDI) tof mass spectrometry was used for the confirmation of hapten number in synthesized antigen. As application of MAb, the MAbs against ginsenosides and glycyrrhizin have been prepared resulting in the development of two new techniques that we named the eastern blotting method and the knockout extract preparation. In eastern blotting technique, glycosides like ginsenosides and glycyrrhizin separated by silica gel TLC were blotted to PVDF membrane that was treated with a NaIO4 solution followed by BSA resulted in glycoside-BSA conjugate on a PVDF membrane. The blotted spots were stained by MAb. Double staining of eastern blotting for ginsenosides using antiginsenoside Rb1 and Rg1 MAbs promoted complete identification of ginsenosides in Panax species. The immunoaffinity concentration of glycyrrhizin was determined by immunoaffinity column conjugated with antiglycyrrhizin MAb resulting in the glycyrrhizin-knockout extract, which was determined by the synergic effect with glycyrrhizin on NO production using the cell line.

Journal ArticleDOI
TL;DR: Two flow methods, based on flow-injection analysis and on multicommutated flow analysis, were compared with regard to their use for the determination of total selenium in infant formulas by hydride-generation atomic absorption spectrometry and it was concluded that the MCFA-based method exhibited a better performance.
Abstract: Two flow methods, based, respectively, on flow-injection analysis (FIA) and on multicommutated flow analysis (MCFA), were compared with regard to their use for the determination of total selenium in infant formulas by hydride-generation atomic absorption spectrometry. The method based on multicommutation provided lower detection and quantification limits (0.08 and 0.27 μg L−1 compared to 0.59 and 1.95 μ L−1, resp.), higher sampling frequency (160 versus. 70 samples per hour), and reduced reagent consumption. Linearity, precision, and accuracy were similar for the two methods compared. It was concluded that, while both methods proved to be appropriate for the purpose, the MCFA-based method exhibited a better performance.

Journal ArticleDOI
TL;DR: The role as carbon source for seedling development was indicated considering that both classes of compounds were similarly consumed in the seeds and that no selective consumption of compounds could be detected.
Abstract: The major secondary metabolites and fatty acids occurring in the seeds of Virola surinamensis were monitored by GC-MS during germination and seedling development. The role as carbon source for seedling development was indicated considering that both classes of compounds were similarly consumed in the seeds and that no selective consumption of compounds could be detected.

Journal ArticleDOI
TL;DR: W Whole-cell, time lapse images are demonstrated to show the ability to transform live cells into dynamic laboratories to monitor temporal and spatial endosomal pH of receptor-bound nanosensors.
Abstract: This review captures the use of live cells as dynamic microlaboratories through implementation of labeled nanoparticles (nanosensors) that have both sensing and targeting functions. The addition of 2,4-e-dinitrophenol-L-lysine (DNP) as a FceRI targeting ligand and 4-mercaptopyridine (4-MPy) as a pH-sensing ligand enables spatial and temporal monitoring of FceRI receptors and their pH environment within the endocytic pathway. To ensure reliability, the sensor is calibrated in vivo using the ionophore nigericin and standard buffer solutions to equilibrate the external [H(+)] concentration with that of the cell compartments. This review highlights the nanosensors, ability to traffic and respond to pH of receptor-bound nanosensors (1) at physiological temperature (37°C) versus room temperature (25°C), (2) after pharmacological treatment with bafilomycin, an H(+) ATPase pump inhibitor, or amiloride, an inhibitor of Na(+)/H(+) exchange, and (3) in response to both temperature and pharmacological treatment. Whole-cell, time lapse images are demonstrated to show the ability to transform live cells into dynamic laboratories to monitor temporal and spatial endosomal pH. The versatility of these probes shows promise for future applications relevant to intracellular trafficking and intelligent drug design.

Journal ArticleDOI
TL;DR: The levels of trace elements in hair from children living in Dar es Salaam have been analysed and there were no big differences between the concentration levels of the essential elements inhair samples collected from the children which might indicate the same food consumption habits.
Abstract: The work presented in this paper is part of the study which aims at determining the levels of elements in hair of children in Tanzania as a bioindicator of their nutrition and health. In this paper, the levels of trace elements in hair from children living in Dar es Salaam have been analysed. The analysis was carried out by long and short irradiation INAA at the reactor centre of the Institute of Nuclear Physics, Rez Czech Republic. 22 samples were collected from children living at Kiwalani about 12 km from Dar es Salaam city and 16 samples from children living at Mlimani, the main campus of University of Dar es Salaam. A total of 34 elements were found in the hair of the children. There were no big differences between the concentration levels of the essential elements in hair samples collected from the children which might indicate the same food consumption habits.

Journal ArticleDOI
TL;DR: This issue presents ten papers, which describe either a specific analytical method for specific types of natural products, the use of natural compounds to aid analytical developments, or modern techniques for the analysis of metals in food stuffs and food quality control.
Abstract: This special issue is aimed at collecting together recent developments in the field of natural product analysis. This issue covers methodologies and applications as diverse as secondary metabolite identification to the detection of metals in food stuffs. The chemistry of natural products has gained prominence not only due to the on-going search for new bioactive substances but also in related areas such as food chemistry and chemical ecology. We feel that this special issue represents some of the wide ranging research currently performed in this diverse area and this is exemplified by the affiliations of the authors of the papers included which is made up of chemists, biochemists, biologists, physicists, toxicologists, physiologists, pharmaceutists, and geochemists. What all of these researchers have in common, despite their wide ranging backgrounds, is the need to make use of the powerful techniques of analytical chemistry to analyze natural compounds in complex matrices. Thus, this special issue is dedicated to all the readers that would like to apply analytical chemistry for natural products analysis. This issue presents ten papers, which describe either a specific analytical method for specific types of natural products, the use of natural compounds to aid analytical developments, or modern techniques for the analysis of metals in food stuffs and food quality control (a growing area of interest). The article by L. de S. Ferreira et al. describes the use of hyphenated techniques to determine fatty acids in a species of seaweed from the Fernando de Noronha archipelago. In addition, a second paper has used SRTXRF analysis as a technique to determine several inorganic species within the same archipelago. Both papers contribute to an increased understanding of adsorption and accumulation of such natural elements by algae in that specific area. V. S. A. Devi and V. K. Reddy's paper presents a methodology for spectrophotometric determination of iron(II) and cobalt(II) using 2-hydroxi-1-naphthaldehyde-p-hydroxybenzoichydrazone which can then be applied for the analyses of biological and water samples that contain these metals. The paper by G. C. Lopes et al. reports the preliminary estimation of the stability of the dried extract from the bark of Guazuma ulmifolia Lam. (“Mutamba”). Thermogravimetry analysis along with HPLC were used in the study. The results can be used as a chemical marker in the quality control of dried extracts of G. ulmifolia. The study by M. F. Zampa et al. is the first report of the antimicrobial peptide from the skin of the Phyllomedusa hypochondrialis frog and its incorporation into nanostructured layered films in conjunction with nickel-tetrasulfonated phthalocyanines. The film was used as a biosensor to detect dopamine, a neurotransmitter associated with diseases such as Alzheimer's and Parkinson's. S. B. A. Barros et al. demonstrate the exploitation of the polyelectrolytic behavior of natural cashew gum (Anacardium occidentale L.), found in northeast Brazil, as a component of a nanocomposite electrode. The performance of the electrodes was evaluated by the determination of dopamine. The paper by H. Tanaka et al. presents matrix-assisted laser desorption/ionization (MALDI) mass spectrometry for the confirmation of the hapten number in synthesized antigens. Two unique applications using MAb, Eastern blotting, and knockout extract have been introduced in this paper. The Eastern blotting method has great potential applications for the wide range of natural products. The article of S. R. de Moraes et al. highlights the use of Lippia sidoides Cham. (also known as alecrim pimenta), native to northeastern Brazil and northern Minas Gerais, and their essential oils. The oxygenated monoterpene 1,8-cineole was the major constituent, followed by isoborneol and bornyl acetate. The chemical composition of essential oils described in this paper differs from that described in the literature for L. sidoides found in its native environment. The paper of M. J. Kato et al. demonstrates the GC-MS monitoring of the major secondary metabolites and fatty acids occurring in the seeds of Virola surinamensis, during germination and seedling development. The authors conclude that the germination of V. surinamensis seeds and the seedling development are processes in which both fatty acids and secondary metabolites (lignans, isoflavonoids and juruenolides) are equally consumed in the seeds indicating their potential physiological role as energy and carbon sources. The article of P. J. Gates and N. P. Lopes describes the application of negative ion chip-based nanospray tandem mass spectrometry for the analysis of flavonoid aglycones. The methodology is tested by the analysis of a crude green tea extract, where the expected flavonoids were readily identified. Norberto P. Lopes Ernani Pinto Michael Niehues Paul J. Gates Ricardo Vessecchi