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#28470986   2017/05/04 Save this To Up

Nickel(II)-assisted enantiomeric differentiation and quantitation of tadalafil by direct electrospray ionization mass spectrometry.

A facile method based on electrospray mass spectrometry was established and validated for the differentiation of enantiomeric tadalafil isomers without using chiral chromatographic separation. The enantiomers were coupled with a chiral selector to form diastereomeric complex ions. Nickel-tadalafil complexes, [Ni(II) (tadalafil)(l-Trp)-H](+) , produced a characteristic fragment ion at m/z 524 by loss of 1-methyl-1,6-dihydropyrazine-2,5-dione via collision-induced dissociation. The relative abundance of this fragment ion to the precursor contributed to differentiate tadalafil enantiomers, and energy-resolved product-ion spectra were applied to determine the molar composition of tadalafil in the mixture (R,R and S,S) as well. In addition, the other two forms of stereomeric isomers of tadalafil (R,S and S,R) could be also distinguished and analyzed by this method. The method was validated in different types of mass spectrometers (AB quadrupole time-of-flight and Bruker ion trap) and also verified by a chiral high-performance liquid chromatography coupled with quadrupole time-of-flight. The chiral determination of tadalafil using MS method proved to be rapid (1-min run time for each sample) and to have the same accuracy and precision comparable to chiral liquid chromatography mass spectrometry methods. This method provides an alternative to commonly used chromatographic technique for chiral determination and is particularly useful in rapid screening in enantioselective synthesis and enantiomeric impurity detection in pharmaceutical industry. Copyright © 2017 John Wiley & Sons, Ltd.

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Cholesterol Cholesteryl E Fontana-Masson Stain Kit Fontana-Masson Stain Kit Trichrome Stain Kit (Mod Trichrome Stain Kit (Mod Epidermal Growth Factor ( Epidermal Growth Factor ( Growth Differentiation Fa Growth Differentiation Fa Human Growth and Differen Human Growth and Differen Human Growth and Differen

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#28043285   2017/01/03 Save this To Up

[Determination of relative elements of hard metal in workplace air and urine by inductive coupled plama].

Objective: To establish a rapid detection method regarding the air conditions of workplace and the workers' urine included Tungsten, Cobalt, Nickel, Titanium, Cadmium, Manganese, Lead and its compounds based on inductively coupled plasma mass spectrometry (ICP-MS) . Methods: The experiment adopts ICP-MS to deter-mine those metals in workshop air and workers urine, evaluate the detection's limitation, the precision and accuracy of the method. Using the membrane filter and urine freeze - dried metal standard material to verify this method. Results: Each element of correlation coefficient was greater than 0.999. The recovery rate of air samples was 91.6%~104.6%, within-batch RSD precision was 1.41%~3.50%, between-run precision was 1.28%~4.31%, urine samples recovery rate was 93.0%~102.6%, within - batch RSD precision was 1.25%~3.56%, between - run precision was 1.58%~4.67%, According to the method every element was within the scope of the standard reference, it was also showed that the established method is accurate and reliable. Conclusion: ICP-MS is an effective and feasible method to detect the workshop air and the workers' urine which included Tungsten, Cobalt, Nickel, Titanium, Cadmium, Manganese, Lead and its compounds.

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#23899322   2013/08/27 Save this To Up

Sustainable design of high-performance microsized microbial fuel cell with carbon nanotube anode and air cathode.

Microbial fuel cells (MFCs) are a promising alternative energy source that both generates electricity and cleans water. Fueled by liquid wastes such as wastewater or industrial wastes, the microbial fuel cell converts waste into energy. Microsized MFCs are essentially miniature energy harvesters that can be used to power on-chip electronics, lab-on-a-chip devices, and/or sensors. As MFCs are a relatively new technology, microsized MFCs are also an important rapid testing platform for the comparison and introduction of new conditions or materials into macroscale MFCs, especially nanoscale materials that have high potential for enhanced power production. Here we report a 75 μL microsized MFC on silicon using CMOS-compatible processes and employ a novel nanomaterial with exceptional electrochemical properties, multiwalled carbon nanotubes (MWCNTs), as the on-chip anode. We used this device to compare the usage of the more commonly used but highly expensive anode material gold, as well as a more inexpensive substitute, nickel. This is the first anode material study done using the most sustainably designed microsized MFC to date, which utilizes ambient oxygen as the electron acceptor with an air cathode instead of the chemical ferricyanide and without a membrane. Ferricyanide is unsustainable, as the chemical must be continuously refilled, while using oxygen, naturally found in air, makes the device mobile and is a key step in commercializing this for portable technology such as lab-on-a-chip for point-of-care diagnostics. At 880 mA/m(2) and 19 mW/m(2) the MWCNT anode outperformed the others in both current and power densities with between 6 and 20 times better performance. All devices were run for over 15 days, indicating a stable and high-endurance energy harvester already capable of producing enough power for ultra-low-power electronics and able to consistently power them over time.

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#17884143   2007/10/22 Save this To Up

Increase of platinum group element concentrations in soils and airborne dust in an urban area in Germany.

Since 1993, all new cars sold in the European Union had to be fitted with catalytic converters. Undoubtedly, these measures brought about a great progress concerning traffic emission controls. However, this technology also led to new emissions. A rapid accumulation of the catalytic active noble metals Pt, Pd, and Rh in the environment was observed and concern arose about potential environmental and health risks. This work aimed at a contribution to a monitoring of platinum group element (PGE) emission and accumulation by comparing analytical data, all generated in 1999 and in 2005 in an urban area in Germany. Oriented at the 1999 sampling strategy, soil and airborne dust samples were taken in 2005 at the same sampling sites located mainly close to heavily used roads in the region of Braunschweig. For the enrichment of the analytes, conditioned soil samples as well as loaded glass fiber filters from air sampling were transferred to the nickel sulphide fire assay. For analyses, the ICP-MS technique was applied. High Pt, Pd, and Rh concentrations were detected especially in top soil layers (0-2 cm) directly at the roadsides or on center strips. At one road outside the city, where traffic moved with a constant speed of about 80 km/h, maximum concentrations in soil were found to be 50.4 microg/kg for Pt, 43.3 microg/kg for Pd, and 10.7 microg/kg for Rh. PGE concentrations were the highest close to that road and exponentially declined with growing distance. At a second road, where vehicles run with a constant speed of 50 km/h, the highest concentrations were detected in the center strip soil: 88.9 microg/kg (Pt), 77.8 microg/kg (Pd), and 17.6 microg/kg (Rh). At a third crowded street in the centre of Braunschweig with stop and go traffic, the highest soil concentrations were determined, namely 261 microg/kg for Pt, 124 microg/kg for Pd and 38.9 microg/kg for Rh. The sampling of airborne dust at this roadside revealed for Pt 159 pg/m(3) air or 1730 microg/kg dust, for Pd 37.8 pg/m(3) air or 410 microg/kg dust, and for Rh 10.0 pg/m(3) air or 110 microg/kg dust. A comparison of analytical results of 2005 with those of 1999 revealed a distinct increase of PGE concentrations in soils closely along heavy traffic roads by a factor of 2.1 to 8.9; once even a factor of 15 was determined. The findings also document, that especially Pt and Rh concentrations were elevated in airborne dust.

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#17270379   2007/03/27 Save this To Up

Automated approach to couple solubility with final pH and crystallinity for pharmaceutical discovery compounds.

The design and validation of a novel high-throughput system for thermodynamic solubility determination requiring only 5 mg of sample is described. The system uses a sintered nickel filter assembly to recover excess solids from saturated solutions for rapid crystallinity assessment via powder X-ray diffraction (PXRD). Moreover, the system measures the pH of filtrates to provide a final pH value with the solubility measurement. The limit of detection for the UV-vis plate reader used on this system is approximately 0.001 mg/ml, while the practical upper limit is approximately 3 mg/mL. The solubility measurements of 60 proprietary Pfizer compounds were used to validate the nickel filter assembly against a more conventional polyvinylidenedifluoride (PVDF) filter. Additionally, a comparison was made between a subset of 10 compounds run on the automated system and a more traditional shake-flask method employing HPLC analysis. In both cases, a favorable comparison was obtained.

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#11159776   2001/02/22 Save this To Up

Development of a routine method for the determination of trace metals in whole blood by magnetic sector inductively coupled plasma mass spectrometry with particular relevance to patients with total hip and knee arthroplasty.

Joint-replacement surgery has revolutionized the treatment of osteoarthritis and is still the most effective therapy. A recent clinical trend reintroducing metal-on-metal bearing surfaces has in turn stimulated a requirement for accurate measurement of the concentrations of relevant metals in both pre- and postoperative patients. Thus, there is a need for cost-effective, multielement methods for trace metal analysis in whole blood to monitor possible increases in wear metal concentrations.

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#9322738   1997/10/30 Save this To Up

Characterization of the rpoC gene of Streptomyces coelicolor A3(2) and its use to develop a simple and rapid method for the purification of RNA polymerase.

The Streptomyces coelicolor rpoC gene, that encodes the beta' subunit of RNA polymerase, was isolated using the Escherichia coli rpoC gene as a hybridization probe. Comparison of the predicted amino acid sequence of the S. coelicolor beta' subunit to those characterized from other bacteria revealed three distinct subfamilies of beta' subunits, one of which consists of the S. coelicolor subunit and those from Mycobacterium leprae and Mycoplasma genitalium. Using site-directed mutagenesis, the carboxy terminus of the S. coelicolor beta' subunit was modified to contain six histidine residues. The histidine-tagged gene, rpoCHIS, was used to replace the wild-type allele in the chromosome of S. coelicolor and S. lividans. These strains were unaffected in growth and sporulation, demonstrating that the histidine-tagged RNA polymerase was competent to carry out all essential in-vivo functions. During a 1-day procedure, highly purified RNA polymerase was obtained by nickel-NTA agarose affinity chromatography followed by heparin-sepharose chromatography. Using in-vitro run-off transcription assays, the affinity purified RNA polymerase was shown to initiate transcription correctly from the S. lividans galP1 and galP2 promoters, and the Bacillus subtilus veg and ctc promoters. An extension of this procedure yielded highly-purified core RNA polymerase. To facilitate introduction of the rpoCHIS allele into other genetic backgrounds, a mutation in the adjacent gene, rpoB (rifA), conferring rifampin-resistance, was isolated in S. coelicolor to provide a genetic marker to follow transfer of the rpoCHIS allele. The use of this affinity chromatography procedure, in combination with the ability to introduce the rpoCHIS allele into different Streptomyces strains by transformation, will greatly facilitate the in-vitro analysis of transcription in members of this genus.

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#9341052   1997/10/20 Save this To Up

Microchannel electrophoretic separations of DNA in injection-molded plastic substrates.

Microfabricated electrophoretic separation devices have been produced by an injection-molding process. The strategy for producing the devices involved solution-phase etching of a master template on a silicon wafer, followed by electroforming more durable injection-molding masters in nickel from the silicon master. One of the nickel electroforms was then used to prepare an injection mold insert, from which microchannel chips in an acrylic substrate were mass-produced. The microchannel devices were used to demonstrate high-resolution separations of double-stranded DNA fragments with total run times of less than 3 min. Run-to-run and chip-to-chip reproducibility was good, with relative standard deviation values below 1% for the run-to-run data and in the range of 2-3% for the chip-to-chip comparisons. Such devices could lead to the production of low-cost, single-use electrophoretic chips suitable for a variety of separation applications, including DNA sizing, DNA sequencing, random primary library screening, and rapid immunoassay testing.

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#8971610   1997/03/24 Save this To Up

Rapid, highly sensitive gradient narrow-bore high-performance liquid chromatographic determination of suramin and its analogues.

A high-performance liquid chromatography (HPLC) method for the determination of suramin, its precursors and analogues in aqueous solutions and in plasma samples with advantages compared to earlier methods is described. Due to the method's high sensitivity (detection limit of suramin in plasma samples: 7 ng/ml; in aqueous solutions: 5 ng/ml) and selectivity (suramin tR: 7.05 min, precursor amine 2 tR: 4.68 min), it is possible to analyze degradation products, impurities and possible metabolites of suramin besides suramin. Tetrabutylammonium hydrogensulfate (TBAHS) (5 mM) is used as ion-pairing reagent in a mixture of 36% methanol and 0.02 M phosphate buffer pH 6.5 is used as the mobile phase. After sample injection, a linear gradient from 36 to 62.9% methanol is run. A C8 stationary phase (100 x 2.1 mm I.D.) is used and ultraviolet (UV) detection at 238 nm is applied. Plasma extraction is performed with tetrabutylammonium bromide (pH 8.0) and acetonitrile. This procedure allows the determination of suramin and its precursor amine 2 in the range of 0.05-400 micrograms/ml with high precision [relative standard deviation of peak areas at 0.05 microgram/ml: 2.10% (n = 5)] and nearly complete recovery (> 96.5%). Because of the high flexibility of the chromatographic system and subsequently the universality of the method, the analysis of a broad range of suramin analogues is possible. The result of the purity check of two suramin analogues is given.

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#2617292   1990/03/05 Save this To Up

Determination of nickel in urine with graphite furnace AAS using Zeeman correction.

We have developed a rapid and direct method for determining urine nickel. The urine specimen is diluted (1 + 1) with 2.0% v/v nitric acid and 0.001% v/v Triton X-100 and absorbance measurements are made with Zeeman-effect graphite furnace atomic absorption. The method is sensitive enough to be used to evaluate "normal" subjects for baseline studies or to evaluate environmental or other nonoccupational exposure to nickel. The characteristic mass (pg/0.0044A.s) is 26 pg, which is comparable to that obtained for aqueous solutions. The observed absorbance is linear up to about 100 micrograms l-1, after which the calibration curve departs from linearity. Procedures are described to rigorously exclude nickel contamination. We evaluated precision and accuracy with a U.S. National Bureau of Standards urine reference material. SRM 2670, with an informational nickel value of 70 micrograms l-1, and with a multielement water reference material, SRM 1643b, with a certified nickel value of 49 ng g-1. Within- and among-run standard deviations for SRM 2670 were calculated to be 9.0 and 2.45 micrograms l-1, respectively, and 2.1 and 1.1 micrograms l-1 for SRM 1643b. The detection limit, calculated as 3 SD of a "low" concentration urine, is about 1.1 micrograms l-1. The proposed method was applied to the determination of nickel in urine of 258 workers in a magnet manufacturing plant, and the data obtained support the usefulness of urine nickel for biological monitoring.

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