Gene/Protein Disease Symptom Drug Enzyme Compound
Pivot Concepts: Gene/Protein Disease Symptom Drug Enzyme Compound   Target Concepts: Gene/Protein Disease Symptom Drug Enzyme Compound

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Query: EC:2.7.10.2 (focal adhesion kinase)
44,029 document(s) hit in 31,850,051 MEDLINE articles (0.00 seconds)

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.
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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 new time-based flow injection on-line solid phase extraction method for chromium(VI) and lead determination using flame atomic absorption spectrometry was developed. The use of hydrophobic poly-chlorotrifluoroethylene (PCTFE)-beads as absorbent in on-line preconcentration system was evaluated. Effective formation of ammonium pyrrolidine dithiocarbamate complexes and subsequently retention in PCTFE packed column, was achieved in pH range 1.0-1.6 and 1.5-3.2 for Cr(VI) and Pb(II) ions, respectively. The sorbed analyte was efficiently eluted with isobutyl-methyl-ketone for on-line FAAS determination. The proposed packing material exhibited excellent chemical and mechanical resistance, fast kinetics for adsorption of Cr(VI) and Pb(II) permitting the use of high sample flow rates at least up to 15mLmin(-1) without loss of retention efficiency. For a preconcentration time of 90s, the sample frequency was 30h(-1), the enhancement factor was 94 and 220, the detection limit was 0.4 and 1.2mugL(-1), while the precision (R.S.D.) was 1.8% (at 5mugL(-1)) and 2.1% (at 30mugL(-1)) for chromium(VI) and lead, respectively. The applicability and the accuracy of the developed method were estimated by the analysis spiked water samples and certified reference material NIST-CRM 1643d (Trace elements in water) and NIST-SRM 2109 (chromium(VI) speciation in water).
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PMID:Determination of chromium(VI) and lead in water samples by on-line sorption preconcentration coupled with flame atomic absorption spectrometry using a PCTFE-beads packed column. 1907 15

The selective catalytic reduction (SCR) of NO(x) with C3H6 was studied in the presence of oxygen. The double wash-coat monolith catalysts for SCR comprised a lower layer of Au (or Pt)/Al2O3 and a upper layer of zeolites. The catalytic performance of the double wash-coated catalyst was remarkably improved to broaden the temperature window. The Au and Pt particles were dispersed uniformly on the monolith with particle sizes range of 3 approximately 5 nm and 5 approximately 10 nm, respectively. The catalyst binders used were colloidal silica, potassium silicate and tetraethyl orthosilicate, and the best catalyst activity was achieved with using colloidal silica as a binder. The zeolites used for the catalyst upper layer were MCM-41, FER, Y5.3-Zeolite and ZSM5, among which the NH4-ZSM5-coated catalyst showed the highest activity. The experimental results confirmed the promising potential of the double wash-coat, monolith catalyst for SCR of NO(x) with C3H6 due to the effective combination of noble metal monolith catalyst with zeolite for the removal of NO(x) by SCR with hydrocarbons.
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PMID:Activity of double wash-coat monolith catalyst with noble metals and zeolites in selective catalytic reduction of NO(x) with C3H6. 1919 44

In this work a LC-MS/MS method for the determination of two quaternary ammonium growth regulators (chlormequat and mepiquat) in food is reported. The separation was based on hydrophilic interaction liquid chromatography (HILIC) without the use of ion-pair reagents. A gradient elution of acetonitrile and formic acid/ammonium formate buffer from 60 to 40% acetonitrile was enough to achieve a resolution >1.5 in less than 4.0min. The HILIC system was coupled to a triple quadrupole mass spectrometer equipped with a heated electrospray probe (H-ESI) providing sub-pg LODs in SRM mode. A straightforward sample treatment (SPE C18 clean-up) was enough to provide MLODs at low ppb levels when analysing a range of food samples that covered different kinds of matrices such as fresh fruit, vegetables, fruit juices, baby food, bread, coffee and beer. Chlormequat was found in seven samples (0.8-126ng/g) but mepiquat was only detected in bread and coffee samples (0.9-166ng/g).
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PMID:Analysis of chlormequat and mepiquat by hydrophilic interaction chromatography coupled to tandem mass spectrometry in food samples. 1932 94

Simvastatin and atorvastatin belong to the group of hypolipidemic drugs, more exactly to the second generation of inhibitors of microsomal 3-hydroxy-3-methylglutaryl-coenzyme A (HMG-CoA) reductase. They induce a significant reduction in total cholesterol, low-density lipoprotein cholesterol and plasma triglycerides, therefore they are widely used in the treatment of hypercholesterolemia even of its severe form-familiar hypercholesterolemia. Simvastatin and atorvastatin as the most widely used statins in clinical treatment and their hydroxy-acid/lactone forms were determined by means of UPLC in connection with triple quadrupole mass spectrometer. Deuterium labeled reference standard compounds were used as internal standards for the quantitation. Separation was performed on Acquity BEH C18 (100 mm x 2.1 mm, 1.7 microm) using gradient elution by mobile phase containing acetonitrile and ammonium acetate pH 4.0, which is convenient in order to prevent interconversion of analytes. ESI in positive mode was used for the ionization of all compounds. Two SRM (selected reaction monitoring) transitions were carefully optimized for each analyte in order to get high sensitivity and selectivity. SPE on Discovery DSC-18 was used as a sample preparation step. Intra-day precision was generally within 10% RSD, while inter-day precision within 15% RSD. Method accuracy expressed as recovery ranged from 75 to 100%. The method was validated with the sensitivity reaching LOQ 0.08-5.46 nmol/l and LOD 0.01-1.80 nmol/l in biological samples. Atorvastatin, simvastatin, its metabolites and hydroxy-acid/lactone forms were monitored in human serum and in lipoprotein fractions (LDL, HDL and VLDL) at patients with end stage renal diseases.
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PMID:Ultra high performance liquid chromatography tandem mass spectrometric detection in clinical analysis of simvastatin and atorvastatin. 1954 Jan 75

This chapter considers the use of a variety of approaches to assess either the bioavailability or the bioaccessibility of metals in soil. The bioavailability of metals from soils is considered with respect to a series of single-extraction methods, including the use of ethylenediaminetetraacetic acid (EDTA), acetic acid, diethylenetriaminepentaacetic acid (DTPA), ammonium nitrate, calcium chloride and sodium nitrate. Then, a procedure for the recovery of metals using a three-stage sequential extraction protocol is described. Two alternate approaches for assessing the environmental health risk to humans by undertaking in vitro gastrointestinal extraction (also known as the physiologically based extraction test, PBET) are considered. Finally, two acid digestion protocols that allow the pseudo-total metal content of samples to be assessed are provided. In all cases details of how the different approaches can be performed are provided, including the specific reagents required (and their preparation), details of the different extraction and acid digestion protocols to be followed and suitable analytical details to allow the measurement of metals by inductively coupled plasma mass spectrometry (ICP-MS) with/without a collision/reaction cell. A detailed Notes section provides experimental details to guide the reader through some of the practical aspects of the procedures. Finally, some experimental results are provided as evidence of the suitability of the approaches described including single-extraction data, using EDTA and acetic acid, for metals in CRM BCR 700. In addition, in vitro gastrointestinal extraction data are provided for metals in CRM SRM 1570A (spinach leaves). The influence of time on the intestinal fluid phase on the recovery of metals in CRM SRM 1570A (spinach leaves) and CRM INCT-TL-1 (tea leaves) is investigated, as well as the repeatability in terms of recovery of metals from soil over a 3-week period by in vitro gastrointestinal extraction.
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PMID:Heavy metal bioavailability and bioaccessibility in soil. 1988 77

Analysis of chromium in Mentha piperita and the soil where it is cultivated was done. The capacity of soil for chromium immobilization and the capacity of M. piperita L., to control its uptake were analyzed by spiking the soil with standard solutions of Cr(III). For each concentration three acidity levels: natural, one unit below and one above its natural acidity (pH(2)=6, pH(1)=5 and pH(3)=7) were tested. Three-stage sequential extraction was performed (I stage: 1M ammonium-acetate, II stage: 0.1M hydroxylamine-chlorohydrate and III stage: 0.2/0.2M oxalic acid/ammonium-oxalate mixture). The chromium content in the extracts was obtained after the measurements by GFAAS. The results (expressed in mgL(-1)), at pH(1), pH(2) and pH(3), respectively, were as follows: I stage: 4.64-10.93, 0.79-5.78 and 0.26-5.26; II stage: 1.14-15.99, 0.76-20.31 and 0.67-20.64; III stage: 0.67-20.64, 19.17-100.76 and 19.17-116.05. A high potential of the soil for chromium immobilization was observed. In parallel, soil and plant samples were prepared by microwave-assisted acid digestion for total chromium determination. By analysis of SRMs (NIST SRM 2711 - Montana II Soil, NIST SRM 8433 - Corn Bran and NIST SRM 1547 - Peach Leaves) good recoveries (72.7-115.3%) were obtained. Additionally, iron and manganese oxides and hydroxides were recognized as matrix components of special importance for mobility of chromium species within a soil structures so, the determination of Mn and Fe was done too.
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PMID:Determination of chromium in Mentha piperita L. and soil by graphite furnace atomic absorption spectrometry after sequential extraction and microwave-assisted acid digestion to assess potential bioavailability. 1991 18

Centrifuged urine, internal standard (promazine), and ammonium formate buffer are mixed in an autosampler vial to achieve a 10-fold dilution of the specimen. Without additional pretreatment, 10 microL of the sample is injected onto a C18 reverse phase column for gradient analysis with ammonium formate/acetonitrile mobile phases. Drugs in the column eluent become charged in the ion source using positive electrospray atmospheric pressure ionization. Pseudomolecular drug ions are analyzed by a hybrid triple quadrupole linear ion trap mass spectrometer operated with a 264-drug selected ion monitoring (SRM) acquisition method that includes an information-dependant acquisition (IDA) algorithm.
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PMID:Broad spectrum drug screening using liquid chromatography-hybrid triple quadrupole linear ion trap mass spectrometry. 2007 72

A ThermoFinnigan sheath liquid flow capillary electrophoresis-mass spectrometry system designed for coupling via a co-axial interface was coupled through an adapted via an alternative, commercially available interface for orthogonal sampling. The affordable, reversible structural alterations made in the commercial LC-MS interface resulted in improved analytical performance. The results of a conventional capillary electrophoresis (CE) method using a commercial co-axial source to determine antioxidant phenolic acids present in virgin olive oil, were compared with those obtained by using a modified orthogonal sampling position. In both cases, separations were done using a 10 mM ammonium acetate/ammonium hydroxide buffer solution at pH 10.0 and a constant applied voltage of 25 kV. The operating variables for the mass spectrometry interface were re-optimized for the modified orthogonal orientation. This allowed the sheath liquid, sheath gas flow rates and capillary voltage to be lowered with respect to the co-axial coupling configuration. In addition, the orthogonal sampling position provided a higher selectivity by effect of ion sampling excluding larger droplets-with an increased momentum along the axis-which were drained through the sink at the bottom of the ion source. Also, the new configuration facilitated sample ionization, improved electrospray stability and led to stronger signals as a result. The new system was validated in terms of precision (repeatability), linearity, and limits of detection and quantification. A comparison of the validation data with the results previously obtained by using a commercial co-axial configuration revealed the adapted orthogonal sampling position to provide better repeatability in both migration times and relative peak areas (<1% and 7% respectively with n=15 replicates), a good linear range (with levels in the microgram-per-litre region) and lower limits of detection-especially for the compounds detected with the lowest sensitivity when co-axial ESI was used, as HFA, GEN, FER and VAN finding LOD among 24-3.0 microg L(-1) respectively.
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PMID:Advantages of using a modified orthogonal sampling configuration originally designed for LC-ESI-MS to couple CE and MS for the determination of antioxidant phenolic compounds found in virgin olive oil. 2060 34

A simple and powerful method has been developed for the rapid and selective determination of Te(IV) and Te(VI), employing dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry using palladium as permanent modifier. Under acidic conditions pH 1, only Te(IV) can form a complex with ammonium pyrrolidine dithiocarbamate (APDC) and therefore be extracted into fine droplets of carbon tetrachloride (extraction solvent) which are dispersed with ethanol into the water sample solution. After centrifugation, Te(IV) was determined in the sedimented organic phase while Te(VI) remained in the aqueous phase. Total inorganic tellurium was determined after the reduction of the Te(VI) to Te(IV). Te(VI) was calculated as the difference between the measured total inorganic tellurium and Te(IV) content. The effective parameters for improving the efficiency of microextraction process were investigated by using experimental and central composite designs. Under optimal conditions the enrichment factor was 125 and the calibration graph was linear in the range of 0.015-1 ng mL(-1) with detection limit and characteristic mass of 0.004 ng mL(-1) and 0.033 pg, respectively. The relative standard deviation for 0.5 ng mL(-1) of tellurium measurement was 3.6% (n=6) at ash and atomization temperature, 900 and 2600 degrees C, respectively. The recoveries of spiked Te(IV) and Te(VI) to the environmental water samples were 89.6-101.3% and 96.6-99.1%, respectively. The accuracy is also evaluated by applying the proposed method to certified reference material (NIST SRM 1643e), for which the result was in a good agreement with the certified values reported for this CRM (95% confidence level).
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PMID:Speciation and determination of ultra trace amounts of inorganic tellurium in environmental water samples by dispersive liquid-liquid microextraction and electrothermal atomic absorption spectrometry. 2068 11


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