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Query: EC:2.7.10.2 (
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In this preliminary study the feasibility of a modified spark source was investigated as a method of rapidly dissolving solid conductive samples in aqueous media prior to analysis by atomic spectroscopy. The spark source, originally designed for spark emission spectroscopy in air, was modified by the installation of a spark ablation vessel. This spark ablation vessel was designed for spark ablating samples in aqueous solution, such as deionised water. Samples such as mild steel and brass were ablated in 5-10 ml of deionised water for 2-30 s producing a colloidal suspension. The suspension was readily dissolved by adding 100 mul of concentrated
HCl
or HNO(3). In this paper the spark ablation vessel is described as well as some of the properties of spark ablation in aqueous solutions. Spark ablation rates on mild steel were measured with respect to spark ablation parameters such as applied current (power), polarity and spark time. Using mild steel as a test sample, spark ablation rates varied from 40 mug s(-1), with 2.5 A of applied current, to 70 mug s(-1) with 10 A of applied current to the electrodes. The feasibility of using this technique for analysing trace levels (mug g(-1)) of elements in solid samples was also demonstrated for elements such as Ni in brass with inductively coupled plasma mass spectrometry (ICP-MS). Quantification of selected elements (Cr, Ni, Mn and Cu) in a certified alloy (
SRM
663) and a non-certified stainless steel showed good agreement between the measured values using spark ablation and the accepted values.
...
PMID:Rapid dissolution of metal in aqueous media using a modified commercial spark source unit. 1896 75
A sensitive and rapid method for the determination of lanthanum, europium and ytterbium by inductively coupled plasma atomic emission spectrometry (ICP-AES) after solid-liquid extraction with microcrystalline naphthalene was developed. Analytes could be quantitatively adsorbed on tribromoarsenazo-cetylpyridinium bromide-naphthalene (TBA-CPB-naphthalene) packed in a column and determined by ICP-AES after desorption with 3 moll(-1)
HCl
. The effect of various experimental parameters, such as pH, reagent amounts, naphthalene concentrations and diverse ions, on the determination of interesting elements were investigated in detail. Under the optimized experimental conditions, the detection limits of this method for La(3+), Eu(3+) and Yb(3+) were 1.3-8.6 ngml(-1), and the relative standard deviations obtained for nine replicate determinations at a concentration of 0.5 mugml(-1) were 1.4-2.2%. The proposed method has been applied in the analysis of NIES CRM No. 8 vehicle exhaust particulates and GBW 07602 GSV-1 bush branches and leaves for La, Eu and Yb, and La in NIST
SRM
1752 citrus leaves samples; the analytical results were in good agreement with reference values.
...
PMID:Preconcentration of lanthanum, europium and ytterbium with tribromoarsenazo-cetylpyridinium bromide supported on microcrystalline naphthalene and their determinations by inductively coupled plasma atomic emission spectrometry. 1896 49
This paper shows the influence of different sample storage protocols, on the chemiluminescence signal of some metal ions. The storage protocols studied were: acid addition (
HCl
or HNO(3)) and no reagent addition to filtered and refrigerated (T=4 degrees C) samples. Light emission was produced for the chemiluminescence reaction between luminol and hydrogen peroxide in buffer carbonate conditions (pH 10.8) catalysed by Cr(III), Co(II) and Cu(II). Batch and/or flow modes in different conditions were tested. Fe(II), Fe(III), Ni(II) and Mn(II) did not give chemiluminescence in the studied conditions. A parallel study of sensitivity and selectivity was performed. Then the presence or absence of the masking agent EDTA, added to samples or used in the carrier stream, is assayed. If the samples are acidified with HNO(3), a previous neutralisation is needed using batch mode. The determination of Cr(III) is independent of storage protocol by flow injection (FI) method; however, the determination of Co(II) or Cu(II) or total determination of three metals requires the conditioning of standards. Detection limits achieved are ranged between 0.5 and 2 mug l(-1). For batch mode, detection limits are better for unacidified samples and worse for carbonate-neutralised samples. The influence of storage protocols was validated using standard metal mixtures and calibration solutions. The use of standard reference material (
SRM
(c) 1640) (Trace elements in natural water) corroborates the previous statements and validates the accuracy of the different approaches underlined. This paper demonstrates that it is possible to determine Cr(III) selectively in natural waters.
...
PMID:Influence of water sample storage protocols in chemiluminescence detection of trace elements. 1896 48
An overview of literature data on vapour generation techniques for cadmium and comparison with own experiments by means of several different types of hydride generation-electrothermal atomic absorption spectrometric systems (HG-ETAAS) (batch, semi-batch (SB), continuous-flow (CF) and flow-injection (FI) as well as different gas-liquid separators (GLS) exhibits apparent variations and inconsistency. However, if data for optimal chemical conditions are re-plotted in another coordinates: C(
HCl
) (mol l(-1)) vs. the ratio of reductant-to-acid molar input rates (i.e. millimoles per minute), [BH(4)(-)]:[H(+)], much better consistency of data is revealed: more than half of data are clustered around 0.2-0.3 mol l(-1)
HCl
which appears an optimal acidity at moderate BH(4)(-) concentrations; the tetrahydroborate molar input rates should always be in excess versus the H(+) molar input rates (1.1 to tenfold); relatively high flow rates of argon purge gas are required (>/=120 ml min(-1)); special attention to the blank control at ng l(-1) levels as well as to the construction of gas-liquid separator and vapour transfer lines should be paid. 'Milder' conditions for HG could be provided with some of the examined systems and GLSs, thus minimizing reagent consumption, blanks, vigorous reactions, foaming, aerosol production and drift in measurements: e.g. 0.4 mol l(-1)
HCl
-3% m/v NaBH(4) with the semi-batch system and 0.25 mol l(-1)
HCl
-2% m/v NaBH(4) in continuous flow mode. Experimental system is based on the Transversely Heated Graphite Atomizer coupled with flow injection system FIAS 400. Integrated platforms are treated for permanent modification with Zr (110 mug) or W (240 mug) and then with Ir (8 mug). Temperatures of trapping, pyrolysis and atomization are 350, 500 and 1300 degrees C, respectively. The best overall efficiency of HG, transportation and trapping is 41%. The characteristic mass for peak area measurements is m(o)=2.8 pg and the limit of detection is 0.002 mug l(-1). The long-term stability of characteristic mass (within-day, 8 h) is m(o)=2.8+/-0.1 pg (R.S.D. 4.0%, n=8), whereas the corresponding between-day figures (1 mo) are m(o)=2.8+/-0.2 pg (R.S.D. 6.6%, n=6). The linear range is 0.002-0.12 mug l(-1) with a sample loop of 1.8 ml, being strongly impaired with smaller sample volumes in FI mode. The sample throughput rate is 10 h(-1) with the semi-batch system. Applications to real human and bovine urine samples and CRMs of sea water (CASS-3), river water (SLRS-1 and SLRS-3) and urine (
SRM
2670) are presented.
...
PMID:Hydride generation atomic absorption spectrometry with different flow systems and in-atomizer trapping for determination of cadmium in water and urine-overview of existing data on cadmium vapour generation and evaluation of critical parameters. 1896 33
The single extractions with 15 extractants (agents) (H(2)O, KCl, NH(4)Cl, NH(4)F, CaCl(2), BaCl(2), CuCl(2), LaCl(3), Na(2)S(2)O(4), (NH(4))(2)C(2)O(4), Na(4)P(2)O(7), NTA, EDTA, DTPA,
HCl
), the optimised BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and the solid phase extraction (SPE) by the chelating ion-exchanger Iontosorb Salicyl (cellulose resin containing covalently bound salicylic acid functional groups) were used for the partitioning of Al in very acid soil samples taken from an area influenced by acid mine solutions. The precision, accuracy and repeatibility for all steps of the optimised BCR SEP were checked on the various reference materials (CRM 483 sewage sludge amended soil, CRM BCR 701 freshwater sediment,
SRM
2710 and
SRM
2711 Montana soils). Also the new indicative values of the optimised BCR SEP fractional Al concentrations were obtained for these reference materials. The aluminium amounts obtained by the used extraction procedures were valuated and discussed from the aspect of the Al concentration in the plants (grass) growing on the same studied soils. The aluminium toxicity indexes (ATI) calculated for the studied soils, the BaCl(2) and acetic acid soil extracts and the grass stems and roots were used for the assessment of the Al toxicity to the plants. The ATI value was defined as the ratio of the nutrient cations (Ca, Mg, K, Na) concentration sum to the Al concentration. The flame atomic absorption spectrometry (LOQ=0.2mgl(-1)) and the inductively coupled plasma optical emission spectrometry (LOQ=0.03mgl(-1)) were used for the aluminium quantification.
...
PMID:Free aluminium extraction from various reference materials and acid soils with relation to plant availability. 1897 Aug 73
A biosorption procedure for preconcentration-separation of nickel(II) and silver(I) at trace levels on Bacillus sphaericus-loaded Chromosorb 106 (BSLC106) has been presented in this work. The conditions like pH, amounts of microorganism, eluent type, etc. for the quantitative adsorption of the analyte ions on BSCL106 column were investigated. The analyte ions were quantitatively recovered and desorbed at pH range of 6.0-7.0 and 10 mL of 1M
HCl
, respectively. The effects of various cationic and anionic interferences on the recoveries of nickel(II) and silver(I) were studied. The detection limits for nickel(II) and silver(I) are 1.42 and 1.05 microg L(-1), respectively. The accuracy of the developed procedure was tested by analyzing NIST
SRM
2711 Montana soil and GBW 07310 Stream sediment certified reference materials. The proposed enrichment-separation procedure was successfully applied to the determination of analytes in natural water, black tea, tobacco, soil and sediment samples with satisfactory results.
...
PMID:Column solid-phase extraction of nickel and silver in environmental samples prior to their flame atomic absorption spectrometric determinations. 1897 95
Our understanding of the innate immune response in the horse has been limited by a lack of definitive data concerning cell signaling in response to microbial products. Toll-like receptors (TLRs) recognize conserved molecular motifs of microbes and elicit immune responses through their coupling with intracellular adaptor molecules, particularly MyD88 and TRIF. To provide a more definitive characterization of TLR signaling in the horse, the objectives of this study were to: (1) characterize the responses of equine monocytes to TLR ligands that signal through MyD88, TRIF or both in other species, and (2) determine the profiles of gene expression initiated utilizing these adaptor molecules. Monocytes were used to establish concentration response curves for Escherichia coli lipopolysaccharide (LPS; TLR4 ligand) and N-palmitoyl-S-[2,3-bis(palmitoyloxy)-(2RS)-propyl]-[R]-cysteinyl-[S]-seryl-[S]-lysyl-[S]-lysyl-[S]-lysyl-[S]-lysine x 3
HCl
(Pam(3)
CSK
(4); TLR2 ligand) based on expression of procoagulant activity (PCA) and production of tumor necrosis factor-alpha (TNF-alpha); effects of polyinosine-polycytidylic acid (Poly I:C; TLR3 ligand) were determined by quantifying expression of mRNA for interferon-beta (IFN-ss). Expression of genes associated with the MyD88- (TNF-alpha, IL-1ss, IL-6 and IL-10) and TRIF-dependent pathways (IFN-ss, IP-10, RANTES and TRAF1) were measured at intervals spanning 20 h. LPS and Pam(3)
CSK
(4) induced significantly higher expression of TNF-alpha, IL-1ss, and IL-10 than did Poly I:C. Poly I:C induced significantly higher expression of IFN-ss, IP-10 and RANTES than did either the TLR2 or TLR4 ligands. High concentrations of E. coli LPS did not significantly increase expression of genes associated with the TRIF-dependent pathway. The results of this study suggest that equine monocytes utilize a common intracellular pathway in response to TLR2 and TLR4 ligands, but a distinct pathway in response to TLR3 ligands.
...
PMID:Differential induction of MyD88- and TRIF-dependent pathways in equine monocytes by Toll-like receptor agonists. 1901 56
A simple solid phase extraction procedure for speciation of selenium(IV) and selenium(VI) in environmental samples has been proposed prior to graphite furnace atomic absorption spectrometry. The method is based on the solid phase extraction of the selenium(IV)-ammonium pyrrolidine dithiocarbamate (APDC) chelate on the Diaion HP-2MG. After reduction of Se(VI) by heating the samples in the microwave oven with 4moll(-1)
HCl
, the system was applied to the total selenium. Se(VI) was calculated as the difference between the total selenium content and Se(IV) content. The experimental parameters, pH, amounts of reagents, eluent type and sample volume were optimized. The recoveries of analytes were found greater than 95%. No appreciable matrix effects were observed. The adsorption capacity of sorbent was 5.20mgg(-1) Se (IV). The detection limit of Se (IV) (3sigma, n=11) is 0.010mugl(-1). The preconcentration factor for the presented system was 100. The proposed method was applied to the speciation of selenium(IV), selenium(VI) and determination of total selenium in natural waters and microwave digested soil, garlic, onion, rice, wheat and hazelnut samples harvested various locations in Turkey with satisfactory results. In order to verify the accuracy of the method, certified reference materials (NIST
SRM
2711 Montana Soil, NIST
SRM
1568a Rice Flour and NIST
SRM
8418 Wheat Gluten) were analyzed and the results obtained were in good agreement with the certified values. The relative errors and relative standard deviations were below 6 and 10%, respectively.
...
PMID:Speciation of selenium(IV) and selenium(VI) in environmental samples by the combination of graphite furnace atomic absorption spectrometric determination and solid phase extraction on Diaion HP-2MG. 1907 60
A rapid and efficient closed vessel microwave-assisted extraction (MAE) method based on acidic leaching was developed and optimized for the extraction of total mercury (Hg), inorganic mercury (Hg(2+)) and methylmercury (CH(3)Hg(+)) from fish tissues. The quantitative extraction of total Hg and mercury species from biological samples was achieved by using 5molL(-1)
HCl
and 0.25molL(-1) NaCl during 10min at 60 degrees C. Total Hg content was determined using inductively coupled plasma mass spectrometry (ICP-MS). Mercury species were measured by liquid chromatography hyphenated with inductively coupled plasma mass spectrometry (LC-ICP-MS). The method was validated using biological certified reference materials ERM-CE464, DOLT-3, and NIST
SRM
-1946. The analytical results were in good agreement with the certified reference values of total Hg and CH(3)Hg(+) at a 95% confidence level. Further, accuracy validation using speciated isotope-dilution mass spectrometry (SIDMS, as described in the EPA Method 6800) was carried out. SIDMS was also applied to study and correct for unwanted species transformation reactions during and/or after sample preparation steps. For the studied reference materials, no statistically significant transformation between mercury species was observed during the extraction and determination procedures. The proposed method was successfully applied to fish tissues with good agreement between SIDMS results and external calibration (EC) results. Interspecies transformations in fish tissues were slightly higher than certified reference materials due to differences in matrix composition. Depending on the type of fish tissue, up to 10.24% of Hg(2+) was methylated and up to 1.75% of CH(3)Hg(+) was demethylated to Hg(2+).
...
PMID:Robust microwave-assisted extraction protocol for determination of total mercury and methylmercury in fish tissues. 1908 17
A slurry sampling inductively coupled plasma mass spectrometry (ICP-MS) method has been developed for the determination of As, Cd, and Hg in cereals using flow injection chemical vapor generation (VG) as the sample introduction system. A slurry containing 6% m/v flour, 0.7% m/v thiourea, 0.4 microg mL(-1) Co(II), and 2.5% v/v
HCl
was injected into a VG-ICP-MS system for the determination of As, Cd, and Hg without dissolution and mineralization. Because the sensitivities of the elements studied in the slurry and that of aqueous solution were quite different, a standard addition method and an isotope dilution method were used for the determination of As, Cd, and Hg in selected cereal samples. The influences of vapor generation conditions and slurry preparation on the ion signals were reported. The effectiveness of the vapor generation sample introduction technique in alleviating various spectral interferences in ICP-MS analysis has been demonstrated. This method has been applied for the determination of As, Cd, and Hg in NIST
SRM
1567a Wheat Flour reference material, NIST
SRM
1568a Rice Flour reference material, and cereal samples obtained from local market. The As, Cd, and Hg analysis results of the reference materials agreed with the certified values. The method detection limits estimated from standard addition curves were about 0.10, 0.16, and 0.07 ng g(-1) for As, Cd, and Hg, respectively, in the original cereal samples.
...
PMID:Slurry sampling flow injection chemical vapor generation inductively coupled plasma mass spectrometry for the determination of As, Cd, and Hg in cereals. 1960 66
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