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131.
Bhavesh Babulal Gabani Suresh P. Sulochana Vinay Kiran Umesh Todmal Ramesh Mullangi 《Biomedical chromatography : BMC》2019,33(11)
A liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) method has been developed and validated for the quantification of tunicamycin in rat plasma as per regulatory guideline. Chromatography of tunicamycin and the IS in the processed plasma samples was achieved on an X‐Terra phenyl column using a binary gradient (mobile phase A, acetonitrile and mobile phase B, 5 mm ammonium formate) elution at a flow rate of 0.6 ml/min. LC–MS/MS was operated under the multiple reaction monitoring mode using the electrospray ionization technique in positive ion mode and the transitions of m/z 817.18 → 596.10, 831.43 → 610.10, 845.29 → 624.10, 859.23 → 638.10 and 309.24 → 163.20 were used to quantitate homologs A–D and the IS, respectively. The total chromatographic run time was 4.5 min. The correlation coefficient (r2) was >0.99 for all homologs with accuracy 90.7–107.4% and precision 0.74–15.1%. The recovery of homologs was 78.6–90.2%. No carryover was observed and the matrix effect was minimal. Tunicamycin four homologs were found to be stable on the bench‐top for 6 h, for up to three freeze–thaw cycles, in the injector for 24 h and for 1 month at ?80 ° C. The applicability of the validated method has been demonstrated in a rat pharmacokinetic study. 相似文献
132.
133.
Ravi Kiran Kaja K. V. Surendranath P. Radhakrishnanand J. Satish P. V. V. Satyanarayana 《Chromatographia》2010,72(5-6):441-446
A novel, sensitive, stability indicating RP-LC method has been developed for the quantitative determination of deferasirox, its related impurities in both bulk drugs and pharmaceutical dosage forms. Efficient chromatographic separation was achieved on a C18 stationary phase with simple mobile phase combination delivered in an isocratic mode and quantitation was by ultraviolet detection at 245 nm. The mobile phase consisted of buffer, acetonitrile and methanol (50:45:5, v/v) delivered at a flow rate of 1.0 mL min?1. Buffer consisted of 10 mM potassium dihydrogen orthophosphate monohydrate, pH adjusted to 3.0 by using orthophosphoric acid. In the developed LC method the resolution (R s ) between deferasirox and its four potential impurities was found to be greater than 2.0. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for deferasirox and its four impurities. This method was capable to detect all four impurities of deferasirox at a level of 0.002% with respect to test concentration of 0.5 mg mL?1 for a 10 μL injection volume. The inter- and intra-day precision values for all four impurities and for deferasirox was found to be within 2.0% RSD. The method showed good and consistent recoveries for deferasirox in bulk drugs (98.3–101.1%), pharmaceutical dosage forms (100.2–103.1%) and for its all the four impurities (99.7–102.1%). The test solution was found to be stable in methanol for 48 h. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in acid stress hydrolysis. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.95%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness. 相似文献
134.
A simple and convenient method for the synthesis of 1‐dialkylaminocarbothioic acid S‐[(2,3‐epithio)propyl] ester was developed by the reaction of 1‐dialkylaminocarbodithioic acid‐sodium salt with 1‐chloro‐2,3‐epoxypropane in water‐methanol mixture at room temperature. An intermediate was isolated and characterized, based on which a possible mechanism was proposed. 相似文献
135.
alpha/beta-Hybrid peptides are prepared from amino acids with proteinogenic side chains on the basis of the concept of "alternating chirality", involving D-Phe and a beta3-hVal. Through the extensive NMR, CD, and MD studies, robust left-handed 11/9-mixed helices were identified in these peptides in CDCl3 solutions, wherein the 11/9-mixed helix was observed even in a small peptide with three residues. 相似文献
136.
Kumaraswamy G Padmaja M Markondaiah B Jena N Sridhar B Kiran MU 《The Journal of organic chemistry》2006,71(1):337-340
[reaction: see text] An efficient protocol has been developed using D-(2R)-Oppolzer sultam as a chiral auxiliary for generating anti/syn diastereomers with high enantiopurity and utilized in the efficient synthesis of natural product belactosin C and their synthetic congeners. It has been observed that a variation in the stoichiometry of the Lewis acid led to a difference in anti/syn selectivity. 相似文献
137.
S. Shanmughapriya G. Seghal Kiran Joseph Selvin T. Anto Thomas C. Rani 《Applied biochemistry and biotechnology》2010,162(3):625-640
Marinobacter sp. (MSI032) isolated from the marine sponge Dendrilla nigra was optimized for the production of extracellular cellulolytic enzyme (CMCase) by submerged fermentation. Initial experiments
showed that the culture medium containing 1% maltose as carbon source and 1% peptone and casein as nitrogen source supported
maximal enzyme production at 27 °C and at a pH of 9.0. Further optimization carried out showed the maximal enzyme production
was supported by the presence of 2% NaCl and 10 mM Zn2+ ions in the production media. The production of enzyme cellulase occurred at 48 h of incubation which proved the importance
of this strain for cellulase production in large scale. Further, the enzyme was purified to 12.5-fold with a 37% yield and
a specific activity of 2,548.75 U/mg. The purified enzyme displayed maximum activity at mesophilic temperature (27–35 °C)
and at a broad pH range with optimal activity at pH 9.0. The purified enzyme was stable even at a higher alkaline pH of 12.0
which is greater than the pH stability that has not been reported in any of the cellulolytic isolates studied so far. Thus,
from the present study, it is crucial that, instead of exploring the thermophilic resource that is limited in natural environments,
the mesophilic bacteria that occurs commonly in nature can be added up to the database of cellulolytic bacteria. Thus, it
is possible that a wide diversity of mesophilic bacteria associated with marine sponges opens up a new doorstep for the degradation
of cellulosic waste material for the production of liquid fuels. This is the first report elucidating the prospects of sponge-associated
marine bacterium for the production of extracellular alkaline cellulase. 相似文献
138.
Suryakant B. Sapkal Kiran F. Shelke Bapurao B. Shingate Murlidhar S. Shingare 《中国化学快报》2010,21(12):1439-1442
<正>l-Methyl-3-ethyl imidazolium bromide[meim]Br/basic alumina(Al_2O_3) has been found to promote the cyclocondensation of chloroacetone/chloroethyl acetate with salicylaldehydes under conventional as well as microwave irradiation to yield benzofuran derivatives. 相似文献
139.
Preparation, structure and spasmolytic activities of some derivatives of harmine series of alkaloids
Begum S Imran Hassan S Siddiqui BS Ifzal R Perwaiz S Kiran T Shaheen F Ghayur MN Gilani AH 《Natural product research》2006,20(3):213-227
Keeping in view the interesting chemistry and pharmacological importance of harmine series of bases -- the beta-carboline alkaloids, a number of new derivatives of tetrahydroharmine and harmalol have been prepared and characterized through spectral studies. Some of these derivatives showed spasmolytic activity. It was observed that all the N-acyl tetrahydroharmine derivatives are stable, not labile and no ring opening occurs in these compounds, as reported recently. 相似文献
140.
Sharma GV Reddy KR Krishna PR Sankar AR Narsimulu K Kumar SK Jayaprakash P Jagannadh B Kunwar AC 《Journal of the American Chemical Society》2003,125(45):13670-13671
The C-linked carbo-beta-peptides, oligomers of a new class of C-linked carbo-beta3-amino acids, have been shown to generate mixed 12/10 and 10/12 helices. The design involves use of "alternating chirality" of the epimeric (at the amine center) monomers to control the stability of these helices. The observation of stable 12/10 helix in a tripeptide and 10/12 helix in a tetrapeptide is unprecedented. 相似文献