Showing papers in "Analytical Sciences in 2006"
TL;DR: Gold nanoparticle modified indium tin oxide (ITO) film coated glass electrodes were prepared for the first time through direct electrochemical deposition from 0.5 M H2SO4 containing 0.1 mM HAuCl4 and characterized with AFM.
Abstract: Gold nanoparticle modified indium tin oxide (ITO) film coated glass electrodes were prepared for the first time through direct electrochemical deposition from 0.5 M H2SO4 containing 0.1 mM HAuCl4. The resulting electrode surfaces were characterized with AFM. Cyclic voltammetry and linear sweep voltammetry (LSV) of arsenic(III) on the modified electrodes were performed. After optimization, a LOD of 5 +/- 0.2 ppb was obtained with 60 s deposition at -0.6 V (vs. SCE) in 1 M HNO3 using LSV.
170 citations
TL;DR: Shifts in the peak potentials in cyclic voltammetry, spectral changes in UV absorption titration, an increase in viscosity of DNA and the results of the effect of ionic strength on the binding constant strongly support the intercalation of proflavine into the DNA double helix.
Abstract: The interaction of proflavine with herring sperm DNA has been investigated by cyclic voltammetry and UV-Vis spectroscopy as well as viscosity measurements. Shifts in the peak potentials in cyclic voltammetry, spectral changes in UV absorption titration, an increase in viscosity of DNA and the results of the effect of ionic strength on the binding constant strongly support the intercalation of proflavine into the DNA double helix. The binding constant for the interaction between proflavine and DNA was K = 2.32 (±0.41) × 104 M-1 and the binding site size was 2.07 (±0.1) base pairs, estimated in voltammetric measurements. The value of the binding site size was determined to be closer to that expected for a planar intercalating agent. The standard Gibbs free-energy change is ca. -24.90 kJ/mol at 25°C, indicating the spontaneity of the binding interaction. The binding constant determined by UV absorption measurements was K = 2.20 (±0.48) × 104 M-1, which is very close to the value determined by cyclic voltammetry assuming that the binding equilibrium is static.
121 citations
TL;DR: The speciation studies reveal that metal ion complexation is one of the most important processes in seawater; especially, most bioactive trace metals, such as Fe(III) and Cu, exist as complexes with ligands in dissolved organic matter.
Abstract: The recent development of the chemical speciation of trace metals in seawater is described. The speciation studies reveal that metal ion complexation is one of the most important processes in seawater; especially, most bioactive trace metals, such as Fe(III) and Cu, exist as complexes with ligands in dissolved organic matter. The organic ligands in seawater are characterized with metal ions selected by the HSAB concept. A strong organic ligand, which originates from marine microorganisms, is classified as a hard base including carboxylates. The free organic ligand concentrations in seawater are buffered by complexation with excess amounts of Ca and Mg in seawater. The chemical equilibrium model suggested that the concentrations of bioactive free metal ions are at an optimal level to activities of marine microorganisms. For chemical speciation, it is important to have a better understanding of the ecological roles of trace metals in seawater.
87 citations
TL;DR: It was found that both static quenching and non-radiation energy transfer were the main reasons leading to the fluorescence quench of CBZ and BSA.
Abstract: The interaction between carbamazepine (CBZ) and bovine serum albumin (BSA) was studied using fluorescence spectroscopy (FS) and ultraviolet spectroscopy (UV). The experimental results showed that the CBZ could insert into the BSA and quench the inner fluorescence of BSA by forming the CBZ-BSA complex. It was found that both static quenching and non-radiation energy transfer were the main reasons leading to the fluorescence quenching. The apparent binding constants (K) between CBZ and BSA were found to be 1.8 × 104 (27°C) and 2.8 × 104 (37°C) and the binding site values (n) were 0.97 (27°C) and 1.01 (37°C), respectively. According to the Forster theory of non-radiation energy transfer, the binding distances (r) between CBZ and BSA were 3.6 nm and 3.4 nm at 27°C and 37°C, respectively. The process of the binding was a spontaneous molecular interaction in which entropy increased and Gibbs free energy decreased, indicating that the interaction between CBZ and BSA was mainly driven by the hydrophobic force.
87 citations
TL;DR: A method to determine alpha-, beta- and gamma-hexabromocyclodododecane (HBCD) and tetrabromobisphenol A (TBBPA) in water and sediments was presented using solid phase extraction (SPE) and/or solvent extraction.
Abstract: A method to determine α-, β- and γ-hexabromocyclododecane (HBCD) and tetrabromobisphenol A (TBBPA) in water and sediments was presented using solid phase extraction (SPE) and/or solvent extraction. Recoveries from sediments were approximately 100% for all the chemicals, while recoveries of α-, β- and γ-HBCDs from water were dependent on the extraction method. In the case of dichloromethane (CH2Cl2) extraction, recoveries of α-, β- and γ-HBCD from landfill leachates were 77%, 88% and 92%, respectively. Technical difficulties in HBCD measurement are discussed in terms of the physico-chemical properties of HBCD isomers. The method was applied to landfill samples and marine sediment.
85 citations
TL;DR: The high permeability of monolithic silica columns resulting from the high porosity is shown to be advantageous to generate large numbers of theoretical plates with long capillary columns in high peak-capacity HPLC separations.
Abstract: Monolithic silica columns and their use in high peak-capacity HPLC separations are reviewed. Monolithic silica columns can potentially provide higher overall performance than particle-packed columns based on the variable external porosity and variable through-pore size/skeleton size ratios. The high permeability of monolithic silica columns resulting from the high porosity is shown to be advantageous to generate large numbers of theoretical plates with long capillary columns. High permeability together with the high stability of the network structures of silica allows their use in high-speed separations required for a second-dimension column in two dimensional HPLC. Disadvantages of monolithic silica columns are also described.
77 citations
TL;DR: Solid phase extraction (SPE) is an effective tool for the preconcentration of trace elements and their separation from various sample constituents as mentioned in this paper, and Octadecyl and other alkyl-bonded silica gels are most widely used for these purposes.
Abstract: Solid-phase extraction (SPE) is an effective tool for the preconcentration of trace elements and their separation from various sample constituents. Octadecyl and other alkyl-bonded silica gels are most widely used for these purposes. The fundamentals of the SPE of inorganic ions are reviewed and compared with those of related techniques (liquid-liquid extraction and reversed-phase liquid chromatography). The extraction of ions in the form of chelate compounds, inorganic salts solvated by neutral reagents, and ion-pair compounds is considered. Numerous applications of SPE to the separation and preconcentration of different elements and their species, including on-line combinations with instrumental determination techniques, are described and tabulated.
71 citations
TL;DR: A carbon paste electrode chemically modified with 1-[4-(ferrocenyl ethynyl)phenyl]-1-ethanone (4-FEPEMCPE) was employed to study the electrocatalytic oxidation of L-cysteine using cyclic voltammetry, differential pulsevoltammetry and double potential step chronoamperometry as diagnostic techniques.
Abstract: A carbon paste electrode (CPE) chemically modified with 1-[4-(ferrocenyl ethynyl)phenyl]-1-ethanone (4-FEPEMCPE) was employed to study the electrocatalytic oxidation of L-cysteine using cyclic voltammetry, differential pulse voltammetry and double potential step chronoamperometry as diagnostic techniques. The diffusion coefficient (D = 7.863 x 10(-6) cm2 s(-1)) of L-cysteine was also estimated using chronoamperometry. The electron-transfer coefficient, alpha (= 0.40), for L-cysteine at the surface of 4-FEPEMCPE was determined using cyclic voltammetry technique. It was found that under an optimum pH (= 7.00), the oxidation of L-cysteine at the surface of such an electrode occurred at a potential of about 350 mV less positive than that of an unmodified CPE. The catalytic oxidation peak currents represented a linear dependence on the L-cysteine concentration. Linear analytical curves were obtained in the ranges of 9.0 x 10(-5) - 4.9 x 10(-3) M and 2.0 x 10(-5) - 2.8 x 10(-3) M of L-cysteine with correlation coefficients of 0.9981 and 0.9982 in cyclic voltammetry and differential pulse voltammetry, respectively. The detection limits (2 sigma) were determined to be 9.9 x 10(-6) M and 5 x 10(-6) M with cyclic voltammetry and differential pulse voltammetry, respectively. The influences of twenty other amino acids, such as glutamine, L-glutamic acid, L-glysine, L-histidine, L-isoleucine, L-leucine, L-arginine hydrochloride, L-aspargine, L-aspartic acid, S-carboxy methyl-L-cysteine, L-methionine, L-phenyl alanine, L-proline, L-serine, L-threonine, L-cystine, cysteamine and gluthathione, on the current response of the sensor were examined. The obtained results did not show any influence on the analytical signal of L-cysteine by these amino acids (except for cysteamine). The method was also used for the selective determination of L-cysteine in patient-blood plasma and some pharmaceutical preparations by using standard addition method.
70 citations
TL;DR: Arsenic speciation analysis in marine samples was performed using high performance liquid chromatography (HPLC) with ICP-MS detection and the low power microwave digestion was employed for the extraction of arsenic species from seafood products.
Abstract: Arsenic speciation analysis in marine samples was performed using high performance liquid chromatography (HPLC) with ICP-MS detection. The separation of eight arsenic species viz. arsenite (As(III)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenate (As(V)), arsenobetaine, trimethylarsine oxide (TMAO), arsenocholine and tetramethylarsonium ion (TeMAs) was achieved on a Shiseido Capcell Pak C18 column by using an isocratic eluent (pH 3.0), in which condition As(III) and MMA were co-eluted. The entire separation was accomplished in 15 min. The detection limits for 8 arsenic species by HPLC/ICP-MS were in the range of 0.02 - 0.10 microg L(-1) based on 3sigma of blank response (n=9). The precision was calculated to be 3.1-7.3% (RSD) for all eight species. The method then successfully applied to several marine samples e.g., oyster, scallop, fish, and shrimps. For the extraction of arsenic species from seafood products, the low power microwave digestion was employed. The extraction efficiency was in the range of 52.9 - 112.3%. Total arsenic concentrations were analyzed by using the microwave acid digestion. The total arsenics in the certified reference materials (DORM-2 and TORT-2) were analyzed and agreed with the certified values. The concentrations of arsenics in marine samples were in the range 6.6 - 35.1 microg g(-1).
68 citations
TL;DR: The characteristics (apparatus, manifold design, and operation mode) of multi-syringe flow injections analysis systems are discussed and critically compared to those of flow injection analysis and sequential injection systems.
Abstract: In the present paper, the characteristics (apparatus, manifold design, and operation mode) of multi-syringe flow injection analysis systems are discussed and critically compared to those of flow injection analysis and sequential injection systems. Furthermore, a survey of applications proposed until the present moment is presented, with special emphasis on implementation of in-line sample treatment.
65 citations
TL;DR: The photochemical fishing approach accelerates the throughput, isolating crosslinked complexes and analyzing the structure of the ligand binding site within the protein, using carbene-generating phenyldiazirine for this approach.
Abstract: Photoaffinity labeling enables the direct probing of a target protein through a covalent bond between a ligand and its binding protein, and even a complex formed by weak interactions can be isolated by the method. The photochemical fishing approach accelerates the throughput, isolating crosslinked complexes and analyzing the structure of the ligand binding site within the protein. We used carbene-generating phenyldiazirine for this approach because practical examinations had shown that the phenyldiazirine functioned as the powerful barb on the hook. Improving the synthetic pathways of the photoprobes and using chemoselective-integrated photoreactive units makes possible the easy and rapid preparation of carbene-generating photoreactive probes including the derivatives in peptides, proteins, DNAs, and carbohydrates. This review also shows several recent impacts of photoaffinity labeling, including the in vivo preparation of photoreactive proteins in living cells.
TL;DR: This method was successfully applied to the determinations of iron in a river water sample and of residual chlorine in tap water samples with N,N-diethylphenylenediamine (DPD).
Abstract: Tristimulus colorimetry using a digital still camera (DSC) as a colorimeter has been developed. A photograph of a sample and standard solutions was taken simultaneously with the DSC, and it was transferred to a PC. On the PC, the colors of the sample and of the standard solutions were analyzed and L* (brightness), a* (red-green component), and b* (yellow-blue component) values were determined with laboratory-made software. A dedicated light-box containing white-color LEDs as light source was made of white acrylic to make constant exposure at each photograph. Various settings of the DSC, such as exposure mode, white balance, and so on, that affect analytical figures, were studied with determination of iron with 1,10-phenanthroline. This method was successfully applied to the determinations of iron in a river water sample and of residual chlorine in tap water samples with N,N-diethylphenylenediamine (DPD).
TL;DR: A highly La(III) ion-selective PVC membrane sensor based on N'-(1-pyridin-2-ylmethylene)-2-furohydrazide (NPYFH) as an excellent sensing material was successfully developed and shows good selectivity for La( III) ion with respect to most common cations including alkali, alkaline earth, transition and heavy metal ions.
Abstract: A highly La(III) ion-selective PVC membrane sensor based on N′-(1-pyridin-2-ylmethylene)-2-furohydrazide (NPYFH) as an excellent sensing material was successfully developed The electrode shows a good selectivity for La(III) ion with respect to most common cations including alkali, alkaline earth, transition and heavy metal ions The proposed sensor exhibits a wide linear response with slope of 192 ± 06 mV per decade over the concentration range of 10 × 10-6 - 10 × 10-1 M, and a detection limit of 70 × 10-7 M of La(III) ions The sensor response is independent of pH in the range of 35 - 100 The proposed electrode was applied as an indicator electrode in potentiometric titration of La(III) ion with EDTA
TL;DR: A disposable amperometric immunosensor was studied for the rapid detection of Vibrio cholerae, the causative agent of cholera, employing an indirect sandwich enzyme linked immunosorbent assay (ELISA) principle.
Abstract: A disposable amperometric immunosensor was studied for the rapid detection of Vibrio cholerae (V. cholerae), the causative agent of cholera, employing an indirect sandwich enzyme linked immunosorbent assay (ELISA) principle. Screen-printed electrodes (SPEs) were fabricated (by using commercial and homemade carbon inks), electrochemically characterized and the assay conditions were optimized for capturing antibodies and antigen. Whole cell lysate (WCL) of V. cholerae was used to raise antibodies in rabbits and mice. The antibodies raised against WCL of V. cholerae were found to be specific, and no cross reactivity was observed with other enteric bacteria. 1-Naphthyl phosphate was used as a substrate with the amperometric detection of its enzymatic hydrolysis product 1-naphthol at a potential of +400 mV vs. Ag/AgCl reference electrode. A comparison between the amperometric detection technique and the standard ELISA was made in terms of the total assay time, the amount of biological materials used and the sensitivity of detection. The minimum detection limit of the amperometric immunosensor for V. cholerae was found to be 10(5) cells/ml in 55 min, while ELISA detected 10(6) cells/ml in 4 h.
TL;DR: Multilayered thin films containing poly(allylamine) (PAA) and brilliant yellow (BY) were prepared on a quartz slide by a layer-by-layer (LBL) deposition technique and the UV-visible spectra of the PAA/BY films were sufficiently changed depending upon the pH value of the solution in which the film was immersed.
Abstract: Multilayered thin films containing poly(allylamine) (PAA) and brilliant yellow (BY) were prepared on a quartz slide by a layer-by-layer (LBL) deposition technique. The UV-visible spectra of the PAA/BY films were sufficiently changed depending upon the pH value of the solution in which the film was immersed. The response of the PAA/BY films was very fast (within a second) upon pH change from 9.0 to 5.0, while the response time was ca. 100 s upon pH change from 5.0 to 9.0.
TL;DR: Three simple spectrophotometric methods have been described and successfully applied to assay of olanzapine in its commercial tablets with mean percentage recoveries of 101.23 +/-0.10, 96 +/- 0.10 and 94 +/- 1.04%.
Abstract: Three simple spectrophotometric methods have been described for the assay of olanzapine in its pure and pharmaceutical formulations. The direct method (A) is based on the drug oxidation with excess of N-bromosuccinimide in acidic medium and the two indirect methods (B and C) are based on the oxidation of the drug with excess of N-bromosuccinimide and cerium(IV)sulfate, followed by the reaction of the unconsumed oxidants with celestine blue. The calibration graphs were linear over the range 10 - 120 µg mL-1 (method A), 0.5 - 6.0 µg mL-1 (method B) and 0.6 - 3.0 µg mL-1 (method C). After validation, the proposed methods were successfully applied to assay of olanzapine in its commercial tablets with mean percentage recoveries of 101.23 ± 0.10, 96 ± 0.10 and 94 ± 0.04%. The mechanism of olanzapine oxidation with N-bromosuccinimide was also proposed.
TL;DR: A simple and sensitive high-performance thin-layer chromatography (HPTLC) method has been developed for the quantitative estimation of gatifloxacin and ornidazole in its combined dosage forms.
Abstract: A simple and sensitive high-performance thin-layer chromatography (HPTLC) method has been developed for the quantitative estimation of gatifloxacin and ornidazole in its combined dosage forms. Gatifloxacin and ornidazole were chromatographed on silica Gel 60 F(254) TLC plate using n-butanol:methanol:ammonia (6 M) (8:1:1.5 v/v) as the mobile phase and scanned at 302 nm using a Camag TLC Scanner 3. The R(f) value of gatifloxacin and ornidazole was found to be 0.21 +/- 0.02 and 0.76 +/- 0.04, respectively. The linearity of gatifloxacin and ornidazole were in the range of 100 - 500 ng/spot and 250 - 1250 ng/spot, respectively. The limit of detection was found to be 40 ng/spot for gatifloxacin and 100 ng/spot for ornidazole. The proposed method was applied for the determination of gatifloxacin and ornidazole in combined dosage forms.
TL;DR: A simple and sensitive method based on the formation of micro particles of Ethyl Violet and molybdoarsenate, which gives an apparently homogeneous blue color to the solution, enabling the spectrophotometric determination of arsenic with the detection limit of 4 microg l(-1).
Abstract: In this study, a simple and sensitive method for the determination of arsenic in water samples was developed. The method is based on the formation of micro particles of Ethyl Violet and molybdoarsenate, which gives an apparently homogeneous blue color to the solution. The absorption of the excess dye gradually decreases due to its conversion to a colorless carbinol species under strongly acidic conditions. Consequently, the sufficiently low reagent blank enables the spectrophotometric determination of arsenic with the detection limit of 4 microg l(-1). The coefficient of variation for the spectrophotometry at 50 microg l(-1) was 3.5% (n = 5). Furthermore, it is possible to detect concentrations as low as 10 microg l(-1) of arsenic visually. Our method will be useful as a simple, rapid, and cost-effective field test of arsenic, requiring no complex apparatus or skilled laboratory support.
TL;DR: The design, fabrication and testing of a sliver sensor that could be developed for in vivo use are described and a micro-miniature array of sensing capsules for optical monitoring of pH, potassium and glucose is described.
Abstract: A micro-miniature array of sensing capsules for optical monitoring of pH, potassium and glucose is described. Optode technology translates the respective ionic levels into variable colors of ionophore/dye/polymeric liquid micro-beads stuffed into individual capsules. Glucose is monitored indirectly, by coupling through glucose oxidase (GOX) immobilized in cellulose acetate phthalate (CAP) based microscopic beads that are stuffed into another microcapsule together with pH sensitive optical microscopic beads. The electrolyte and glucose sensing capsules are embedded in a transparent cellulose acetate bar 300 - 500 μm wide and 2 - 2.5 mm long called the sliver sensor that includes also a white capsule made of micro-beads without dye for optical reference. By adding further capsules custom combinations of analytes can be monitored in biomedical and non-biological contexts. In this work, as an example, design, fabrication and testing of a sliver sensor that could be developed for in vivo use are described.
TL;DR: The proposed method was applied to the determination of hydroxylamine in water samples with satisfactory results and the relative standard deviation for 10 determinations was 1.81% and the limit of detection was 0.010 microg mL(-1).
Abstract: A simple, precise and accurate method is proposed for rapid determination of trace amounts of hydroxylamine based on the reaction of hydroxylamine with iodate in acidic media. The reaction of neutral red by the produced nitrite ion was used to monitor the reaction spectrophotometrically at 525 nm by a fixed time method. Hydroxylamine in the range of 0.0400-1.200 microg mL(-1) could be determined. The relative standard deviation for 10 determinations of 0.500 microg mL(-1) hydroxylamine was 1.81% and the limit of detection was 0.010 microg mL(-1). The proposed method was applied to the determination of hydroxylamine in water samples with satisfactory results.
TL;DR: The recognition ability of pteridine derivatives for nucleobases opposite an abasic (AP) site in an oligodeoxynucleotide duplex is enhanced by using a propylene residue (Spacer-C3) as an AP site.
Abstract: The recognition ability of pteridine derivatives for nucleobases opposite an abasic (AP) site in an oligodeoxynucleotide (ODN) duplex is enhanced by using a propylene residue (Spacer-C3) as an AP site. The recognition ability is further enhanced both by attaching methyl groups to a fluorescent ligand and by measuring the fluorescence response at 5 degrees C; 6.2 x 10(6) M(-1) of the binding constant is attained between 2-amino-6,7-dimethyl-4-hydroxypteridine and guanine opposite the AP site in water.
TL;DR: A preconcentration HPLC system with 2,4-dinitrophenylhydrazine with high detection limits for low-molecular-weight carbonyl compounds in drinking water and natural water and applications to commercial mineral water, tap water, river water, pond water and seawater are presented.
Abstract: The aim of this research was to develop a simple procedure for a highly sensitive determination of low-molecular-weight (LMW) carbonyl compounds in drinking water and natural water. We employed a preconcentration HPLC system with 2,4-dinitrophenylhydrazine (DNPH) for the determination of LMW carbonyl compounds. A C-18 reverse-phase preconcentration column was used instead of a sample loop at the sample injection valve. A 0.1 - 5.0 mL portion of the derivatized sample solution was injected with a gas-tight syringe, and a 15% acetonitrile aqueous solution was pushed through the preconcentration column to remove the unreacted excess DNPH, which caused serious interference in the determination of formaldehyde. The detection limits were 1 - 3 nM with a relative standard deviation of 2 - 5% for 20 nM standard solutions (n = 5). The calibration curves were essentially unaffected by coexisting sea salts. Applications to commercial mineral water, tap water, river water, pond water and seawater are presented.
TL;DR: The cloud-point methodology was successfully employed for the preconcentration of heavy metal cations at trace levels from aqueous samples prior to flame atomic absorption spectrometry (FAAS).
Abstract: The cloud-point methodology was successfully employed for the preconcentration of heavy metal cations at trace levels from aqueous samples prior to flame atomic absorption spectrometry (FAAS). Cations were taken into a complex with 8-quinolinol in an aqueous non-ionic surfactant, Triton X-114, medium and concentrated in the surfactant rich phase by bringing the solution to the cloud-point temperature. The preconcentration of only 100 mL of the solution with 1% Triton X-114 and 10(-3) M 8-quinolinol at pH 7.0 gave a preconcentration factor higher than 100 for most cations. Under these conditions, the detection limits of the cloud-point extraction-FAAS system were 0.8 - 15 microg/L.
TL;DR: A rapid sample-digestion method for the determination of toxic metals, cadmium, chromium, and lead, in polyethylene and polyvinyl chloride has been developed by using a microwave oven for household use.
Abstract: A rapid sample-digestion method for the determination of toxic metals, cadmium, chromium, and lead, in polyethylene and polyvinyl chloride has been developed by using a microwave oven for household use. An appropriate amount of the sample taken in a PTFE decomposition vessel was mixed with nitric acid or nitric and sulfuric acids. The vessel was heated in a microwave oven by a predetermined operating program. The digested sample was diluted to a definite volume with water after evaporating most of the nitric acid. The precipitate, if formed, was filtered off by a membrane filter. The metals were determined by ICP-AES. The sample digestion required 5 min (for 20-mg sample) to 25 min (for 60-mg sample). The analytical results obtained for cadmium, chromium, and lead in a polyethylene certified reference material, BCR-680, digested with nitric acid, were in good agreement with the certified values.
TL;DR: NMR measurements coupled with pattern-recognition analysis offer a powerful mixture-analysis tool for latent-feature extraction and sample classification of tea infusions and revealed marker variables that include catechin and theanine peaks.
Abstract: NMR measurements coupled with pattern-recognition analysis offer a powerful mixture-analysis tool for latent-feature extraction and sample classification. As fundamental applications of this analysis for mixtures, the 1H spectra of 176 kinds of green, black, oolong and other tea infusions were acquired by a 500 MHz NMR spectrometer. Each spectrum pattern was analyzed by a multivariate statistical pattern-recognition method where Principal Component Analysis (PCA) was used in combination with Soft Independent Modeling of Class Analogy (SIMCA). SIMCA effectively selected variables that contribute to tea categorization. The final PCA resulted in clear classification reflecting the fermentation and processing of each tea, and revealed marker variables that include catechin and theanine peaks.
TL;DR: The proposed method for the simultaneous separation and preconcentration of trace amounts of copper and zinc ions in an aqueous medium using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) as an analytical reagent has been developed.
Abstract: This work assesses the use of modified natural natrolite zeolite as an adsorptive material for the separation and preconcentration of trace amounts of ions. In this work we investigated the potential of modified natural natrolite zeolite for the simultaneous separation and preconcentration of trace amounts of copper and zinc ions. We have developed a simple, rapid, selective, sensitive and economical method for the simultaneous separation and preconcentration of trace amounts of copper and zinc in an aqueous medium using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) as an analytical reagent. The sorption was quantitative in the pH range 7.5 - 9.5, whereas quantitative desorption occurred instantaneously with 5.0 mL of 2 mol L-1 nitric acid. Linearity was maintained between 0.05 - 6.0 µg mL-1 for copper and 0.02 - 1.5 µg mL-1 for zinc in the final solution. Ten replicate determinations of 1.0 µg mL-1 copper and 0.5 µg mL-1 zinc in a mixture gave mean absorbances of 0.1687 and 0.2788 with relative standard deviations of ±1.2% and ±1.3%, respectively. The detection limits were 0.03 ng mL-1 for Cu(II) and 0.006 ng mL-1 for Zn(II) in the original solution (3 σbl/m). Different parameters, such as the effect of the pH, flow rate, breakthrough volume and interference of a large number of anions and cations, were studied and the proposed method was used for the determination of these metal ions in water as well as standard samples (e.g. Nippon Keikinzoku Kogyo (NKK) CRM, No. 916 and No. 920 aluminum alloy, National Institute for Environment Studies (NIES) No. 1 pepperbush and NIES No. 2 pond sediment). The determination of these metal ions in standard samples showed that the proposed method has good accuracy (recovery > 97%).
TL;DR: The selectivity of each carotenoid changed with the elapsed time and its time evolution was dependent on the carOTenoid component, indicating that the location profile and the content can be important factors to understand the SFE behavior of eachCarotenoids in persimmon peels.
Abstract: The extraction of carotenoids from Japanese persimmon peels by supercritical fluid extraction (SFE), of which the solvent was CO(2), was performed. In order to enhance the yield and selectivity of the extraction, some portion of ethanol (5 - 20 mol%) was added as an entrainer. The extraction temperature ranged from 313 to 353 K and the pressure was 30 MPa. The effect of temperature on the extraction yield of carotenoids was investigated at 10 mol% of the ethanol concentration in the extraction solvent, and a suitable temperature was found to be 333 K among the temperatures studied with respect to the carotenoid yield. With increasing the entrainer amount from 0 to 10 mol% at a constant temperature (333 K), the carotenoid yield in the extraction was improved, whereas the selectivity of the extracted carotenoids was drastically depressed. We also conducted qualitative and quantitative analyses for the carotenoid components in the extract by HPLC, and analyzed the extraction behavior of each individual carotenoid (alpha-carotene, beta-carotene, beta-cryptoxanthin, lycopene, lutein, and zeaxanthin). The selectivity of each carotenoid changed with the elapsed time and its time evolution was dependent on the carotenoid component, indicating that the location profile and the content can be important factors to understand the SFE behavior of each carotenoid in persimmon peels.
TL;DR: A flow injection analysis system was built with a liquid core waveguide spectrophotometric detector using an 80 cm Teflon AF-1600 capillary tube to determine nitrite ion in river water samples.
Abstract: A flow injection analysis system was built with a liquid core waveguide spectrophotometric detector using an 80 cm Teflon AF-1600 capillary tube (2,2-bistrifluoromethyl-4,5-difluoro-1,3-dioxole/tetrafluoroethylene). The system was applied to determine nitrite ion in river water samples. The lower limit of detection for nitrite was 2.1 nmol dm-3 (0.1 ng dm-3 as NO2-) and the relative standard deviation of measurements was typically 0.56% (n = 5) at 0.21 µmol dm-3.
TL;DR: In this article, an optical receiver analog front-end circuit capable of operating at 2.5 Gbps was presented, which integrated both transimpedance amplifier and post limiting amplifier on a single chip.
Abstract: This paper presents the design of an optical receiver analog front-end circuit capable of operating at 2.5 Gbit/s. Fabricated in a low-cost 0.35-/spl mu/m digital CMOS process, this integrated circuit integrates both transimpedance amplifier and post limiting amplifier on a single chip. In order to facilitate high-speed operations in a low-cost CMOS technology, the receiver front-end has been designed utilizing several enhanced bandwidth techniques, including inductive peaking and current injection. Moreover, a power optimization methodology for a multistage wide band amplifier has been proposed. The measured input-referred noise of the optical receiver is about 0.8 /spl mu/A/sub rms/. The input sensitivity of the receiver front-end is 16 /spl mu/A for 2.5-Gbps operation with bit-error rate less than 10/sup -12/, and the output swing is about 250 mV (single-ended). The front-end circuit drains a total current of 33 mA from a 3-V supply. Chip size is 1650 /spl mu/m/spl times/1500 /spl mu/m.
TL;DR: Incorporation of a liquid waveguide capillary flow cell into a flow injection instrument enhances the sensitivity of flow injection analysis with spectrophotometric detection by two orders of magnitude.
Abstract: Incorporation of a liquid waveguide capillary flow cell into a flow injection instrument enhances the sensitivity of flow injection analysis with spectrophotometric detection by two orders of magnitude. Nitrite determination at nM levels has been used to demonstrate the feasibility of this novel technique for trace analysis. Combining the long pathlength spectrophotometry with flow injection analysis, this technique has advantages of low detection limit, good precision and high sample throughput.