Simultaneous chiral and chemoseparation of R-(+)-rabeprazole and related (enantio)impurities was achieved on a cellulose tris-(3,5-dichlorophenylcarbamate) stationary phase chemically bonded to silica gel (Chiralpak IC). A gradient elution was applied in the reverse-phase separation mode. The mobile phase consisted of a mixture of acetonitrile and aqueous phosphate buffer at pH 7. The other operational parameters were flow rate of 1 mL min−1, column temperature of 35 °C and ultraviolet (UV) detection at 282 nm. Quantification limits for R-(+)-rabeprazole and the related impurities ranged in the interval of 0.02–0.03 %. Linear response intervals of 0.02–0.66 % were obtained with UV detection. Validation of the proposed method was achieved according to current regulations in force. For better understanding of the R-(+)-rabeprazole impurity profile, (+)-EMS/MS and
MS/MS detection were also used.
Ultra-performance liquid chromatography coupled with photodiode-array detection has been used to develop a simple, sensitive, and reproducible reversed-phase method for quantitative determination of fingolimod hydrochloride and all possible process-related impurities. Chromatographic separation was achieved on a Waters Acquity BEH C18 (100 mm × 2.1 mm, 1.7 µm) column. The mobile phase was a gradient prepared from potassium dihydrogen phosphate (20 mM) containing 0.1 % (v/v) triethylamine and adjusted to pH 6.5 with trifluoroacetic acid (component A) and 85:15 (v/v) acetonitrile–water (component B); the gradient program (time (min)/% B) was: 0.01/20, 2.0/20, 6.0/75, 9.0/90, 12.0/90, 14.0/20, 16.0/20; the run time was 16 min and fingolimod hydrochloride and its six impurities were well separated. Eluting compounds were monitored at 220 nm. The method was validated for precision, specificity, linearity, limit of detection, limit of quantification, accuracy, and robustness in accordance with International Conference on Harmonization guidelines. Fingolimod hydrochloride was subjected to oxidative, acid, base, hydrolytic, thermal, and photolytic stress, and analysis was conducted to determine the amounts of related impurities formed. 相似文献
A best proximity point theorem explores the existence of an optimal approximate solution, known as a best proximity point, to the equations of the form Tx = x where T is a non-self mapping. The purpose of this article is to establish some best proximity point theorems for non-self non-expansive mappings, non-self Kannan- type mappings and non-self Chatterjea-type mappings, thereby producing optimal approximate solutions to some fixed point equations. Also, algorithms for determining such optimal approximate solutions are furnished in some cases. 相似文献
An efficient PTSA catalyzed synthesis of 2-(N-acyl)aminobenzimidazoles and 2-(N-acyl)aminobenzothiazoles has been described using S-ethylated-N-acylthioureas as substrates and polyethylene glycol as solvent. 相似文献
Multivariable Bernstein functions are used to discover some interesting connections between multivariable completely hyperexpansive weighed shifts and multivariable subnormal weighted shifts. 相似文献
Based on the core structure of Felbinac drug, three series (4a–d, 5a–d and 6a–n) of five membered heterocyclic derivatives containing three heteroatoms were designed and synthesized starting from Felbinac. In the rational design of the target molecules, the biphenyl ring along with the methylene bridge of felbinac was retained while the carboxyl group was substituted with biologically active substituents like 1,2,4-triazole, 1,3,4-thiadiazole and 1,3,4-oxadiazole, with an intent to obtain novel, better and safer anti-inflammatory agents with improved efficacy. The prepared molecules were then investigated for their anti-inflammatory, ulcerogenicity and analgesic activity in experimental animals. The tested compounds exhibited varying degrees of inflammatory activity (25.21–72.87%), analgesic activity (27.50–65.24%) and severity index on gastric mucosa in the range of 0.20–0.80 in comparison to positive control felbinac (62.44%, 68.70% and 1.5, respectively). Among all the prepared compounds, 2-(biphenyl-4-ylmethyl)-5-(4-chlorophenyl)-1,3,4-oxadiazole (6c) emerged as the most potent NSAID compound exhibiting the highest anti-inflammatory activity (72.87% inhibition) and analgesic activity (65.24%) along with the least severity index on gastric mucosa (0.20). Further, molecular docking on cyclooxygenase and in silico ADME-Toxicity prediction studies also supported the experimental biological results and indicated that 6c has a potential to serve as a drug candidate or lead compound for developing novel anti-inflammatory and analgesic therapeutic agent(s) with minimum toxicity on gastric mucosa. 相似文献
A series of diethyl/ethylphenyl {2-(benzo[d]thiazol-2-yl)phenylamino}phosphonates and phosphinates were synthesized under microwave irradiation and neat conditions via Kabachnik-Fields reaction in high yields (80%–93%). The compounds were screened for antimicrobial and antioxidant properties. A few compounds showed effective antibacterial and antifungal activities at MIC value 12.5 μg/mL as compared with the standard at MIC value 6.25 μg/mL. 相似文献
Let us deliberate the question of computing a solution to the problems that can be articulated as the simultaneous equations \({Sx = x}\) and \({Tx = x}\) in the framework of metric spaces. However, when the mappings in context are not necessarily self-mappings, then it may be consequential that the equations do not have a common solution. At this juncture, one contemplates to compute a common approximate solution of such a system with the least possible error. Indeed, for a common approximate solution \({x^*}\) of the equations, the real numbers \({d(x^*, Sx^*)}\) and \({d(x^*,Tx^*)}\) measure the errors due to approximation. Eventually, it is imperative that one pulls off the global minimization of the multiobjective functions \({x \rightarrow d(x, Sx)}\) and \({x \rightarrow d(x, Tx)}\). When S and T are mappings from A to B, it follows that \({d(x, Sx) \geq d(A, B)}\) and \({d(x, Tx) \geq d(A, B)}\) for every \({x \in A}\). As a result, the global minimum of the aforesaid problem shall be actualized if it is ascertained that the functions \({x \rightarrow d(x, Sx)}\) and \({x \rightarrow d(x, Tx)}\) attain the lowest possible value d(A, B). The target of this paper is to resolve the preceding multiobjective global minimization problem when S is a T-cyclic contraction or a generalized cyclic contraction, thereby enabling one to determine a common optimal approximate solution to the aforesaid simultaneous equations. 相似文献
Aldose sugars undergo smooth coupling with enamines, generated in situ from aryl amines and 1,3-diketones, in the presence of 10 mol % of InCl3 in water at 80 degrees C to furnish annulated pyrrole derivatives in relatively good to high yields. The use of InCl3, in combination with water, makes this procedure quite simple, more convenient, and environmentally friendly. 相似文献
This environmentally benign work describes a simple electrochemical sensor constructed with a chemically modified carbon paste electrode (CMCPE) using aloe vera xanthate nanoparticles to detect mercury ions. The characterization and morphology of nanoparticles were thoroughly investigated using modern techniques. The CMCPE efficiently senses the mercury ions. The limit of detection of mercury ions wasexcellent to the order of 0.231 μg mL−1. Real-time sample analysis showed promising results. The recovery range was between 99.4 % and 101.7 %. The activity of CMCPE was commendable even after fifty days. 相似文献