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J. Manjunath Swamy Narendra Kamath Anil Kumar Radha Shekar Nuggehally R. Srinivas Fjalar Kristjansson 《Biomedical chromatography : BMC》2010,24(5):528-534
Sensitivity enhancement via summation of multiple MRM transition pairs is gaining popularity in tandem mass spectrometric assays. Numerous validation experiments describing the assays for two model substrates, clopidogrel and ramiprilat, were performed. The quantitation of clopidogrel was achieved by the summation of transition pairs m/z 322.2 to m/z 212.0 and m/z 322.2 to m/z 184.0, while that of ramiprilat was achieved by the summation of transition pairs m/z 389.2 to m/z 206.1 and m/z 389.2 to m/z156.1. The use of summation approach achieved sensitivities of >2 fold for both compounds as compared with the reported single MRM transition pair assays. The validation experiments addressed some important assay development issues, such as: (a) lack of impact of matrix effect; (b) unequivocal verification of the percentage contribution of each MRM transition pair towards sensitivity; (c) sensitivity enhancement factor achieved by summation approach of MRM transition pairs; and (d) accurate prediction of quality control samples using summation approach vs a single MRM transition pair. In summary, the appropriateness of using two MRM transition pairs for quantitation was demonstrated for both clopidogrel and ramiprilat. Additionally, pharmacokinetic application of the MRM transition pair assays using a summation approach was established for the two compounds. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
13.
A. P. Karande A. K. Fulzele Amrit Prakash Md. Afzal J. P. Panakkal H. S. Kamath 《Journal of Radioanalytical and Nuclear Chemistry》2010,284(2):451-455
Neutron Well Coincidence Counting has been explored as a non destructive assay technique for determining the percentage of
PuO2 in blended mixture of UO2 and PuO2 powders. The method has been applied to MOX blends having PuO2 content varying from 0.4 to 44% for both thermal and fast reactors. The use of Neutron Well Coincidence Counting technique
is validated as a process control step for determining PuO2 content in the fabrication of MOX fuel by comparing it with chemical analysis of sintered pellets. It has been used at Advanced
Fuel fabrication Facility, Bhabha Atomic Research Centre, Tarapur during the manufacture of MOX fuel of various types for
thermal and fast reactors. 相似文献
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The [LiAl(2)(OH)(6)](+) layer obtained from gibbsite-Al(OH)(3) belongs to the layer group symmetry P-312/m. This layer satisfies the defining characteristics of a synthon in that it predicts all the polymorphic modifications of the layered double hydroxides of Li and Al. The various possible ways of stacking these layers can be derived by the systematic elimination of the principal symmetry elements comprising the layer group. This approach yields the complete universe of possible structures. When the 3 axis of the layer is conserved in the stacking, the resultant crystal adopts the structure of the 1H, 2H, or 3R polytypes (H, hexagonal; R, rhombohedral). When the 3 axis is destroyed and the 2/m axis is retained, the crystal adopts monoclinic symmetry and crystallizes in the structures of the 1M(1) or 1M(2) (M, monoclinic) polytypes; the two polytypes differ only in their translational component. Experimentally, gibbsite-based precursors yield the 2H polytype, and bayerite-based precursors yield the 1M polytype. Faulted structures incorporating differently oriented 1M(1) motifs or a mixture of 1M(1) and 1M(2) motifs are also obtained. These stacking faults result in cation disorder along the c axis and produce signature effects on the line shapes of select reflections in the powder X-ray diffraction patterns. This symmetry-guided approach is general and can be extended to other classes of layered solids. 相似文献
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Jack bean urease was immobilized on polyethylenimine-coated cotton cloth by adsorption following by crosslinking with dimethyl suberimidate. Of the various methods used, crosslinking with dimethyl suberimidate was found to stabilize the enzyme with minimal inactivation. Cloth-bound urease showed a shift in pH optimum towards the acidic side without appreciable change in temperature optimum and thermostability. Cloth-bound urease could be used repeatedly for urea hydrolysis without appreciable loss in activity. Alternatively, urease cloth could be stitched in the form of a bag containing ammonia adsorbent and used for urea hydrolysis with simultaneous removal of ammonia. 相似文献
18.
The C-cyanoethylation of the methyl and ethyl ethers of dimethylphenols has been carried out with acrylonitrile in the presence of anhydrous AlCl3 to furnish propionitrile derivatives. The latter on hydrolysis to the corresponding propionic acids followed by cyclization with PPA afforded the appropriate indanones, whose structures have been established on the basis of spectral data and by the formation of 2, 4-DNP derivatives. 相似文献
19.
Kamath Srinivas S. Narayana B. D’Souza Renita Shiny Nayak S. Rashmi Mohan M. P. Dileep B. N. Baburajan A. Ravi P. M. Karunakara N. 《Journal of Radioanalytical and Nuclear Chemistry》2019,322(2):389-397
Tritium concentration was monitored in different water sources collected around Kaiga Nuclear Power plant, India. The concentration was in the ranges?<?1.9–27.4 Bq L?1 (GM?=?4.0 Bq L?1) for groundwater,?<?1.9–42.1 Bq L?1 (GM?=?3.5 Bq L?1) for surface water and in 12.4–42.0 Bq L?1 (GM?=?24.07 Bq L?1) for reservoir water. The concentration values observed in this study are similar to those reported for other PHWR stations of the world. The radiation dose to the public due to ingestion of Tritium through groundwater was computed to be 0.08 μSvy?1.
相似文献20.
Kamath SD Kartha VB Mahato KK 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2008,70(1):187-194
An experimental system for measuring simultaneously photoacoustic (PA) and fluorescence signals is described. The simultaneous measurement of laser induced fluorescence and photoacoustic signals provide a suitable method for the study of different quenching phenomena occurring in fluorescent systems. In this paper we report tryptophan solvation dynamics in water using fluorescence and photoacoustic spectra recorded simultaneously by photoacoustic and fluorescence signals as functions of concentration, indicate that quantum yield is maximum at low concentrations. Also, the energy lost in the fluorescence path of tryptophan, due to different quenching phenomena like self quenching, Resonance energy transfer (RET), solvation relaxation, etc. is clearly seen from the photoacoustic signal intensity which increases as the fluorescence intensity decreases. 相似文献