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11.
12.
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
13.
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
14.
Ram P. Singhal 《Separation & Purification Reviews》2013,42(2):339-398
The recent commercial development of high pressure liquid chromatographic instruments, and the availability of small and uniformly sized resin beads has enhanced the role of column chromatography for the rapid assay of nucleic acid components. A major advancement in the purification and analysis has been due to the recent demonstration that the ion exclusion is more or equally effective than the ion exchange as a separation principle for the resolution of purine and pyrimidine bases, nucleosides, deoxynucleosides and nucleotides1–3. This article deals with the recent applications of separation principles that have been employed for the separation of nucleic acid constituents. The reader is referred to two review articles of Cohn for the earlier works on this subject4, 5. Separations by chromatography and electrophoresis on paper and thin layers are not described here; several monographs and review articles are available in the literature6–12.The reader is also referred to a recent methodological study for the base analysis of ribopolynucleotides by chemical tritium labeling which utilizes two dimensional chromatography on thin layers of cellulose as a separation means13, 14. 相似文献
15.
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.
16.
A simple method for the preparation of enantiopure furo[2,3-b]pyrroles, a rare class of concave bicyclic nitrogen and oxygen heterocycle, in promising yield has been developed. The 3-substituted pyrrolidinediones prepared from (2S,3S)-tetrahydro-3-hydroxy-5-oxo-2,3-furandicarboxylic acid (Garcinia acid) have been cyclized diastereo as well as enantioselectively to furo[2,3-b]pyrroles. The cyclization follows Baldwin’s rule. 相似文献
17.
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
18.
Divya Kumar Vemuri Rambabu Gundla Naresh Konduru Ravindra Mallavarapu Naresh Kumar Katari 《Biomedical chromatography : BMC》2022,36(6):e5363
Favipiravir finished dosage was approved for emergency use in many countries to treat SARS-CoV-2 patients. A specific, accurate, linear, robust, simple, and stability-indicating HPLC method was developed and validated for the determination of degradation impurities present in favipiravir film-coated tablets. The separation of all impurities was achieved from the stationary phase (Inert sustain AQ-C18, 250 × 4.6 mm, 5-μm particle) and mobile phase. Mobile phase A contained KH2PO4 buffer (pH 2.5 ± 0.05) and acetonitrile in the ratio of 98:2 (v/v), and mobile phase B contained water and acetonitrile in the ratio of 50:50 (v/v). The chromatographic conditions were optimized as follows: flow rate, 0.7 mL/min; UV detection, 210 nm; injection volume, 20 μL; and column temperature, 33°C. The proposed method was validated per the current International Conference on Harmonization Q2 (R1) guidelines. The recovery study and linearity ranges were established from the limit of quantification to 150% optimal concentrations. The method validation results were found to be between 98.6 and 106.2% for recovery and r2 = 0.9995–0.9999 for linearity of all identified impurities. The method precision results were achieved below 5% of relative standard deviation. Forced degradation studies were performed in chemical and physical stress conditions. The compound was sensitive to chemical stress conditions. During the study, the analyte degraded and converted to unknown degradation impurities, and its molecular mass was found using the LC–MS technique and established degradation pathways supported by reaction of mechanism. The developed method was found to be suitable for routine analysis of research and development and quality control. 相似文献
19.
Vijayakumar Sekar González-Sánchez Zaira I. Malaikozhundan Balasubramanian Saravanakumar Kandasamy Divya Mani Vaseeharan Baskaralingam Durán-Lara Esteban F. Wang Myeong-Hyeon 《Journal of Cluster Science》2021,32(5):1129-1139
Journal of Cluster Science - Metal oxide nanoparticles (NPs) have gained attention in biomedicine due to their broad spectrum of applications, such as targeted drug delivery, their use as... 相似文献
20.
Anitha Kumary Vidyadharan Divya Jayan T. E. Mary Nancy 《Journal of Solid State Electrochemistry》2014,18(9):2513-2519
A novel electrochemical sensor based on nickel-doped cobalt ferrite nanoparticles (Ni0.1Co0.9Fe2O4)-modified glassy carbon electrode (NCF/GCE) was presented for the sensitive detection of paracetamol. Experimental conditions such as pH, applied potentials and concentration were investigated using cyclic voltammetric and chronoamperometric techniques. The modified electrode exhibited excellent catalytic response towards the oxidation of paracetamol with good reproducibility. The overpotential for oxidation of paracetamol is decreased, and the current response enhanced significantly on the modified electrode in comparison with that of bare electrode. Linear calibration curve is obtained over the range 2 μM to 8,000 μM having a detection limit of 11 nM. The modified electrode facilitated the simultaneous detection of paracetamol, ascorbic acid, and dopamine with good reproducibility. 相似文献