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排序方式: 共有271条查询结果,搜索用时 31 毫秒
1.
Kirtikumar D. Bharwad Priyanka A. Shah Pranav S. Shrivastav Vinay S. Sharma Puran Singhal 《Biomedical chromatography : BMC》2020,34(1):e4708
A rapid, simple and sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method has been developed to quantify fenoprofen, a nonsteroidal anti-inflammatory drug in human plasma for a pharmacokinetic study in healthy subjects. Owing to high levels of protein binding, protein precipitation followed by solid-phase extraction was employed for the extraction of fenoprofen and fenoprofen-d3 (used as internal standard) from 200 μL human plasma. Separation was performed on a BEH C18 (50 × 2.1 mm, 1.7 μm) column using methanol−0.2% acetic acid in water (75:25, v/v) under isocratic elution. Electrospray ionization was operated in the negative mode for sample ionization. Ion transitions used for quantification in the selected reaction monitoring mode were m/z 241/197 and m/z 244/200 for fenoprofen and fenoprofen-d3, respectively. Under the optimized conditions, fenoprofen showed excellent linearity in the concentration range 0.02–20 μg/mL (r2 ≥ 0.9996), adequate sensitivity, favorable accuracy (96.4–103.7%) and precision (percentage coefficient of variation ≤4.3) with negligible matrix effect. The validated method was successfully applied to a pharmacokinetic study of fenoprofen in healthy subjects. The significant features of the method include higher sensitivity, small plasma volume for processing and a short analysis time. 相似文献
2.
Electroanalytical Studies of Chromone Based Ionophores for the Selective Determination of Arsenite Ion 下载免费PDF全文
Neha Gupta Ashok Kumar Singh Shubhrajyotsna Bhardwaj Divya Singhal 《Electroanalysis》2015,27(5):1166-1175
Two chemosensors 4H‐1‐benzopyran‐3‐carboxaldehyde, 4‐oxo‐, 3‐(2‐phenylhydrazone), [I1] and 4H‐1‐benzopyran‐3‐carboxaldehyde, 4‐oxo‐, 3‐[2‐(2,4‐dinitrophenyl)hydrazone], [I2] with hydrazone‐NH group as binding site have been shown excellent selectivity for arsenite ion. It is confirmed by the UV‐vis titration that I2 is more selective than I1. The performance of the coated graphite electrode (CGE) was found to be better than polymeric membrane electrode (PME) in terms of linear range of 4.89×10?7–1.0×10?1 mol L?1, low detection limit of 8.31×10?8 mol L?1 and short response time. The proposed sensors were also used to determine the arsenite ion in different water samples. 相似文献
3.
On the growth and approximation of entire functions represented by Laplace–Stieltjes’ transformation
In the present paper, we obtain the characterization of various growth parameters of an entire function F(s) represented by Laplace–Stieltjes transformation in terms of the rate of decrease of \(E_n ( {F,\beta } ),\)where \(E_n ( {F,\beta } )\) represents the error in approximating the function F(s) by exponential polynomials. 相似文献
4.
Two methods for determining the location of and load level to produce instability of compressed cylindrical shells are presented. The first relates the variation in the wall normal stiffness as a function of applied compressive force to the critical load. It uses the distribution of stiffness over the surface of the shell as a guide to buckle location. The second method associates the local dynamic mass with instability behavior. The test data presented show that either method will give excellent prediction capability from low-load-level data for shells of orthodox form. Neither method appears to apply to spirally stiffened shells. This is thought to be due to the fact that there is a substantial difference between the buckle pattern under axial compression and the imperfection shape induced by the normal displacement which is used to ascertain the wall stiffness and the dynamic mass. 相似文献
5.
Organic ammonium tribromide (OATB), N-methylpyrrolidine-2-one hydrotribromide (MPHT) was found to be an efficient catalyst for the regioselective ring opening of epoxides with various nucleophiles under solvent free conditions. This procedure occurs under neutral and mild reaction conditions with out adding any additive and afforded high yields of products.
6.
Abhaysingh Bhadoriya Priyanka A. Shah Pranav S. Shrivastav Kirtikumar D. Bharwad Puran Singhal 《Biomedical chromatography : BMC》2019,33(8)
A high‐throughput and sensitive ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method has been developed for the determination of terbinafine in human plasma. The method employed liquid–liquid extraction of terbinafine and terbinafine‐d7 (used as internal standard) from 100 μL human plasma with ethyl acetate–n‐hexane (80:20, v/v) solvent mixture. Chromatography was performed on a BEH C18 (50 × 2.1 mm, 1.7 μm) column using acetonitrile–8.0 mm ammonium formate, pH 3.5 (85:15, v/v) under isocratic elution. For quantitative analysis, MS/MS ion transitions were monitored at m/z 292.2/141.1 and m/z 299.1/148.2 for terbinafine and terbinafine‐d7, respectively, using electrospray ionization in the positive mode. The method was validated according to regulatory guidance for selectivity, sensitivity, linearity, recovery, matrix effect, stability, dilution reliability and ruggedness with acceptable accuracy and precision. The method shows good linearity over the tested concentration range from 1.00 to 2000 ng/mL (r2 ≥ 0.9984). The intra‐batch and inter‐batch precision (CV) was 1.8–3.2 and 2.1–4.5%, respectively. The method was successfully applied to a bioequivalence study with 250 mg terbinafine in 32 healthy subjects. The major advantage of this method includes higher sensitivity, small plasma volume for processing and a short analysis time. 相似文献
7.
8.
R. K. Singhal H. Basu M. V. Pimple V. Manisha M. K. T. Bassan A. V. R. Reddy 《Journal of Radioanalytical and Nuclear Chemistry》2014,301(3):805-810
During this work, size fractionation technique “ultra filtration” is used in physical speciation of thorium in organic rich groundwater. Laboratory simulated experiments were carried out to study the physical speciation of thorium in aquatic environment having elevated level of dissolved humus material classified as dissolved organic carbon (DOC). Samples were collected from organic rich environment having DOC in the range of 50–60 µg mL?1. Th(IV) ions are extremely particle reactive having K d value of the order of 105–6, hence to avoid adsorption on suspended particulate matter, spiking of the solution with Th(NO3)4 was carried out in ground water samples after filtering through 450 nm pore size using suction filtration. Particles in dissolved state (colloids) ranging between <450 and >220 nm were separated using suction filtration assembly having a membrane with a pore diameter of 220 nm. Thereafter, solution was sequentially passed through the ultra-filtration membranes having pore diameters of 14 nm [300 k NMWL (nominal molecular weight limit)], 3.1 nm (50 k NMWL), 2.2 nm (30 k NMWL), 1.6 nm (10 k NMWL) and 1.1 nm (0.5 k NMWL) by using “Stirred Ultra-filtration Cells”, operating in concentration mode. Thorium has only one stable oxidation state i.e. IV, under all redox conditions in natural waters and therefore, its speciation is dominated by its interaction with various fractions of DOC. Experimental results show 50–60 % of the spiked Th is in association with fraction enriched with particles of 10 k NMWL (1.6 nm) followed by fraction enriched with particle of 0.5 k NMWL and <220 nm. 相似文献
9.
R. K. Singhal P. K. Sharma M. K. T. Bassan H. Basu A. V. R. Reddy 《Journal of Radioanalytical and Nuclear Chemistry》2011,288(1):149-156
During this work selective separation of uranium from rock phosphate and columbite mineral was done before its quantitative
estimation by using Inductively Coupled Plasma Optical Emission Spectrometery (ICP-OES). Uranium from the rock phosphate and
columubite was extracted by sodium peroxide fusion followed by leaching in 2 M HNO3. To avoid spectral interference in the estimation of uranium by ICP-OES, the selective separation of uranium from the leachate
was carried out by using two different extractants, 30% Tributyl Phophates (TBP) in CCl4 and a equi-volume mixture of Di(2-ethylhexyl) phosphoric acid (D2EHPA) & TBP in petrofin. Uranium was stripped from the organic
phase by using 1 M ammonium carbonate solution. Determination of uranium by ICP-OES was done after dissolving the residue
left after evaporation of ammonium carbonate solution in 4% HNO3. The concentration of the uranium observed in the rock phosphates samples was 40–200 μg g−1 whereas in columbite samples the concentration range was 100–600 μg g−1. Uranium concentration evaluated by ICP-OES was complimented by gamma & alpha spectrometry. Concentration of uranium evaluated
by gamma spectrometry in case of rock phosphate and coulmbite was in close agreement with the uranium content obtained by
ICP-OES. Uranium determination by alpha spectrometry showed only minor deviation (1–2%) from the results obtained by ICP-OES
in case of rock phosphates whereas in case of coulmbites results are off by 20–30%. 相似文献
10.
Kiran Singhal Dharmendra K. Srivastava 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):1673-1678
Abstract Interactions of HgX2 (X = Cl, Br, I, SCN, CN, NCO), SbCl3, TeCl4, and PhTeCl3 with Ph3Sn-O-SiPh3 at room temperature have been found to proceed with the simultaneous cleavage of Sn-O and Si-O bonds, invariably yielding Ph2SnO, Ph3SiX, and the corresponding organo-mercury, -antimony, and -tellurium derivatives. The course of the reactions suggests the instability of the Sn-O-M (M = Hg, Sb, Te) system. GRAPHICAL ABSTRACT 相似文献