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排序方式: 共有332条查询结果,搜索用时 15 毫秒
1.
Harsha K. Tripathy Nair S.V. Manju Sreekanth Dittakavi Ram Murthi Bestha Ramesh Mullangi 《Biomedical chromatography : BMC》2020,34(12):e4953
Larotrectinib is a first-generation tropomyosin kinase inhibitor, approved for the treatment of solid tumors. In this paper, we present a validated dried blood spot (DBS) method for the quantitation of larotrectinib from mouse blood using HPLC–MS/MS, which was operated under multiple reaction monitoring mode. To the DBS disc cards, acidified methanol enriched with internal standard (IS; enasidenib) was added and extracted using tert-butyl methyl ether as an extraction solvent with sonication. Chromatographic separation of larotrectinib and the IS was achieved on an Atlantis dC18 column using 10 mm ammonium formate–acetonitrile (30:70, v/v) delivered at a flow-rate of 0.80 ml/min. Under these optimized conditions, the retention times of larotrectinib and the IS were ~0.93 and 1.37 min, respectively. The total run time was 2.50 min. Larotrectinib and the IS were analyzed using positive ion scan mode and parent–daughter mass to charge ion (m/z) transitions of 429.1 → 342.1 and 474.1 → 267.1, respectively, were used for the quantitation. The calibration range was 1.06–5,080 ng/ml. No matrix effect or carryover was observed. Hematocrit did not influence DBS larotrectinib concentrations. All of the validation parameters met the acceptance criteria. The applicability of the validated method was shown in a mouse pharmacokinetic study. 相似文献
2.
Dinesh Topwal U. Manju Sugata Ray S. Raj D. D. Sarma S. R. Krishnakumar M. Bertolo S. La Rosa G. Cautero 《Journal of Chemical Sciences》2006,118(1):87-92
Disordered Sr2FeMoO6 shows a drastic reduction in saturation magnetization compared to highly ordered samples, moreover magnetization as a function
of the temperature for different disordered samples shows qualitatively different behaviours. We investigate the origin of
such diversity by performing spatially resolved photoemission spectroscopy on various disordered samples. Our results establish
that extensive electronic inhomogeneity, arising most probably from an underlying chemical inhomogeneity in disordered samples, is
responsible for the observed magnetic inhomogeneity. It is further pointed out that these inhomogeneities are connected with
composition fluctuations of the type Sr2Fe1+x
Mo1-x
O6 with Fe-rich (x > 0) and Mo-rich (x < 0) regions.
Dedicated to Prof J Gopalakrishnan on his 62nd birthday. 相似文献
3.
Manju Lata Rao 《Solid State Communications》2004,129(12):781-784
Bulk amorphous Co(100−x)Ptx (0≤x≤50) nano-alloys have been synthesized using high frequency ultrasound, displaying single domain (4-5 nm) behavior wherein weakly exchange-coupled particles lead to a field-dependent resistivity behavior. Magneto-resistivity is correlated to the order-disorder parameter in these powder compacts. The plot of Δρ/ρ0 as a function of reduced magnetization indicates that all the systems are weakly exchange coupled. 相似文献
4.
Manju Rajeswaran Thomas N. Blanton David R. Whitcomb Nicholas Zumbulyadis Brian J. Antalek Scott T. Misture 《Journal of solid state chemistry》2006,179(4):1053-1059
In continuation of our interest in solid-state structures of silver complexes of photographic importance, the structure for silver benzotriazole (AgBZT), has now been obtained. The preferred method for solving crystal structures is via single-crystal X-ray diffraction (XRD). However, for some materials, growing single crystals of appropriate size and quality is often difficult or even impossible. AgBZT is an example of such a silver complex with poor solubility. The usual routes to preparing single crystals using recrystallization from a cooperating solvent resulted in polycrystalline powder samples. We propose a crystal structure for AgBZT, solved from synchrotron X-ray powder diffraction data, using a direct-space Monte Carlo simulated annealing approach. AgBZT crystals are monoclinic, (P21/c), with unit cell dimensions, a=14.8052(3) Å, b=3.7498(4) Å, c=12.3495(12) Å, and β=114.200(6)°. The AgBZT complex is constructed from all three of the Benzotriazole (BZT) nitrogens bonding to a separate silver atom. As a consequence of this bonding mode, the structure is a highly cross-linked, coordination polymer. 相似文献
5.
Sensitive, rapid, and simple spectrophotometric methods were developed for determination of the anticancer drugs vinblastine sulfate (VBS) and vincristine sulfate (VCS), which belong to the class of vinca alkaloids. The first method is based on the reaction of VBS and VCS with diazotized dapsone, forming yellow azo products with absorption maxima at 430 nm. The colored species obey Beer's law in the concentration range of 0.5-24 microg/mL for VBS and 0.5-12 microg/mL for VCS. The second method describes the reaction of VBS and VCS with iron(III) and subsequent reaction with ferricyanide in hydrochloric acid medium to yield blue products with absorption maxima at 750 nm. The Beer's law range for this method is 0.1-4 microg/mL for VBS and 0.5-10 microg/mL for VCS. With both methods, colored species were stable for 1 h. The methods are simple and reproducible and are applied for determination of VBS and VCS in pharmaceutical formulations. Commonly encountered pharmaceuticals added as excipients do not interfere in the analysis and the results obtained in the analysis of dosage forms agree well with the labeled contents. 相似文献
6.
The reaction of gaseous H2S with aqueous ammonium heptamolybdate in the presence of triethylenetetramine (trien) gave a red complex. The complex was recrystallized in hot water and characterized by element analysis and UV, visible, IR, and 1H NMR spectroscopy. PMR has revealed accidental magnetic equivalence, resulting from the proximity of [MoS4]2- species in one complex molecule to the open triethylenetetramine ligand of another molecule. (TrienH2)[MoS4] crystallizes in the orthorhombic crystal system, space group Pca21, a=13.045(2), b=16.461(3), c=13.754(2) , =90, =90, =90°, V=2953.5(9) 3, Z=8, R1=0.0323, wR2=0.0730. The structure consists of the tetrahedral tetrathiomolybdate anions, forming an extended 3D framework in solids due to the interactions with triene cations via Mo-S...H-N hydrogen bonds. 相似文献
7.
A sensitive, rapid, and simple spectrophotometric method is described for the determination of sulfa drugs. The method is based on the formation of a red-colored product by the diazotization of sulfonamides such as sulfathiazole (SFT), sulfadiazine (SFD), sulfacetamide (SFA), sulfamethoxazole (SFMx), sulfamerazine (SFMr), sulfaguanidine (SFG), and sulfamethazine (SFMt), followed by complexation with dopamine in the presence of molybdate ions in (1 + 1) H2SO4 medium. Absorbance of the resulting red product is measured at 490-510 nm, and the product is stable for 2 days at 27 degrees C. Beer's law is obeyed in the concentration range of 0.04-8.0 microg/mL at the wavelength of maximum absorption. The method was used successfully for the determination of some sulfonamides in tablets and eye drops. Common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method offers the advantages of simplicity, rapidity, and sensitivity without the need for extraction or heating. The limits of detection and quantitation were calculated for SFT, SFD, SFA, SFMx, SFMr, SFG, and SFMt. 相似文献
8.
The X-ray crystal structures of a series of lithium quinolates – lithium 8-hydroxyquinolinate (Liq), lithium 2-methyl-8-hydroxyquinolinate (MeLiq), and 2-phenyl-8-hydroxquinolinate (PhLiq), are compared. The substitution at the 2-position of the 8-hydroxyquinoline ligand has significant impact on the aggregation of the lithium complex in the crystalline state. Liq and MeLiq molecules crystallize as hexamers, whereas PhLiq crystallizes as a tetramer. The possible influence of crystal-packing forces on the preferred cluster structure was probed using density functional theory calculations on a systematically varied set of Liq, MeLiq, and PhLiq clusters. For Liq and MeLiq, the observed structures match the most stable computed structures. In the PhLiq case, the observed tetrameric structure is computed to be less stable (+1.2 kcal/mol/monomer) than the lowest energy structure, a hexamer. In this case, solid-state effects probably outweigh small differences in cluster stability. 相似文献
9.
T. Vijay T. Narasimhamurthy H. S. Yathirajan R. S. Rathore P. Nagaraja 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(1):o36-o38
In the crystal structure of the title salt, C7H7Cl2N2O2+·Cl−, the chloride anions participate in extensive hydrogen bonding with the aminium cations and indirectly link the molecules through multiple N+—H⋯Cl− salt bridges. There are two independent molecules in the asymmetric unit, related by a pseudo‐inversion center. The direct intermolecular coupling is established by C—H⋯O, C—H⋯Cl and C—Cl⋯Cl− interactions. A rare three‐center (donor bifurcated) C—H⋯(O,O) hydrogen bond is observed between the methylene and nitro groups, with a side‐on intramolecular component of closed‐ring type and a head‐on intermolecular component. 相似文献
10.
Manju Gupta 《Talanta》2007,71(3):1039-1046
The aim of present work was to optimize the experimental parameters in single drop microextraction under solution immersion (SDME) and headspace (HS-SDME) extraction modes for the determination of periodate using guaifenesine [3-(2′-methoxyphenoxy)-1,2-propane diol] and norephedrine (phenylpropanolamine) as new and alternative reagents for the Malaprade reaction. The reactions were complete within 5 min resulting in the formation of 2-(2′-methoxyphenoxy)-acetaldehyde and benzaldehyde, respectively. SDME/HS-SDME of oxidation products with 2 μl of anisole or 1 μl of toluene, respectively, has permitted the determination of periodate at μg l−1 concentration levels. The results indicated that HS-SDME (range 0.01-10 mg l−1, r2 = 0.9990; limit of detection 1.55 μg l−1) was more sensitive than SDME (range 0.05-50 mg l−1, r2 = 0.9984; limit of detection 3.42 μg l−1), and was inexpensive, rapid and convenient. Tolerance of excess of iodate has permitted the application of this method in the determination of ethylene glycol in motor oil; the average recovery on spiked sample was 98.6% with R.S.D. of 4.2%. 相似文献