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排序方式: 共有121条查询结果,搜索用时 15 毫秒
1.
Validation of LC/MS electrospray ionisation method for the estimation of ursodiol in human plasma and its application in bioequivalence study 总被引:1,自引:0,他引:1
Sundd Singh S Shah H Gupta S Jain M Sharma K Patel H Shah B Thakkar P Patel N Shah R Bhushan Lohary B 《Annali di chimica》2004,94(12):951-959
A novel High Performance Liquid Chromatography-electrospray mass spectrometric method has been developed for the estimation of Ursodiol (Ursodeoxycholic acid)--a bile acid, in human plasma using Ornidazole as internal standard. The methodology involved solid phase extraction of the analyte from human plasma matrix. The chromatographic separation was achieved within seven minutes by an isocratic mobile phase containing 1.0 mM ammonium acetate and Acetonitrile (65:35, v/v), flowing through XTerra MS C18, 100 x 2.1, 3.5 microm analytical column, at a flow rate of 0.2 ml/min. Ion signals were measured in negative mode for Ursodiol and internal standard at m/z 391.3 and 278.1, respectively. A detailed validation of the method was performed as per USFDA guidelines and the standard curves were found to be linear in the range 50.0 ng/ml to 3000.0 ng/ml with the mean correlation coefficient more than 0.99. The absolute recovery was more than 54.90% for Ursodiol and 76.51% for internal standard. Ursodiol was stable for sixty-nine days at -70 degrees C and for eight hours at ambient temperature. After extraction from plasma, the reconstituted samples of Ursodiol were stable in autosampler at 10 degrees C for forty-eight hours. Upon subjecting to three freeze thaw cycles, there was no change in the recovery of the analyte. The integrity of the plasma samples remained unaffected even upon four-fold dilution with drug free human plasma. The method was simple, specific, sensitive, precise, accurate and suitable for bioequivalence and pharmacokinetic studies. It was successfully applied to the pilot bioequivalence study of Ursodiol in male human subjects. 相似文献
2.
This is a corrigendum to our paper, "On a class of prime entire functions", published in Acta Math. Sin., Engl. Ser., 25, 1647-1652 (2009). 相似文献
3.
An efficient method for N-alkylation of diethyl acetamidomalonate (DEAM) is reported. C-Alkenylation was achieved by treating the N-alkenylated DEAM with various electrophiles in the presence of Cs2CO3. RCM reactions of C- and N-alkenylated products gave cyclic amino acid derivatives in good yields. 相似文献
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Anshu Dandia Dinesh Kumar Mahawar Ruchi Sharma Ranveer Singh Badgoti Kuldeep S. Rathore Vijay Parewa 《应用有机金属化学》2019,33(11)
Graphene oxide (GO)‐catalyzed selective synthesis of amides via CSp3–H activation of methylarenes and consequent C–N bond formation with anilines under aqueous medium has been described. Oxygen functionality allied with GO surface played a dual role both as acid catalyst and oxidizing agent to some extent. However, GO has a copious effect on the reaction, shown by a high TOF value with TBHP as co‐oxidant. The decisive role of carboxylic acid functional groups on GO nanosheets in this metal‐free strategy has been confirmed and was monitored by various analytic techniques viz. Fourier transform‐infrared, UV–Vis, Raman and XPS. A plausible mechanism was proposed by control experiments and by the isolation of the intermediate. Over‐oxidation of methylarenes was not detected, and high recyclability of the carbocatalyst with its heterogeneous behavior facilitated the isolation and purification of the desired products. We have further explored the utility of this process for the chemoselective synthesis of benzimidazoles. 相似文献
8.
Vikas Verma Kuldeep Singh Ashok Kumar Devinder Kumar 《Journal of Thermal Analysis and Calorimetry》2013,112(1):339-344
The use of unconventional synthesis methods in the formation of CaO·2Al2O3 (CA2) is justified because it reduces the formation temperature of the compound. CA2 is formed by classical method at temperatures above 1,400 °C. The polymeric precursor method allows a significant temperature decrease in CA2 synthesis reaching temperatures of 1,000 °C. This paper deals with CA2 synthesis by “citrate” method which is often presented as Pechini method, starting from a mixture of citric acid, ethylene glycol and calcium, and aluminum nitrates. A method based on the formation of a polymeric precursor was also used, starting from a mixture of acrylic acid and nitrates of calcium and aluminum. The results showed a net difference in favor of samples obtained from acrylic acid, which by annealing at 800 °C for 1 h, contain pure CA2. The samples obtained from citric acid, after annealing at 800 °C are amorphous. After annealing at 900 °C in all samples CA2 is single phase. 相似文献
9.
A proton-conducting nanocomposite gel polymer electrolyte (GPE) system, [35{(25 poly(methylmethacrylate) (PMMA) + 75 poly(vinylidenefluoride-co-hexafluoropropylene) (PVdF-HFP))?+?xSiO2}?+?65{1 M NH4SCN in ethylene carbonate (EC) + propylene carbonate (PC)}], where x?=?0, 1, 2, 4, 6, 8, 10, and 12, has been reported. The free standing films of the gel electrolyte are obtained by solution cast technique. Films exhibit an amorphous and porous structure as observed from X-ray diffractometry (XRD) and scanning electron microscopy (SEM) studies. Fourier transform infrared spectrophotometry (FTIR) studies indicate ion–filler–polymer interactions in the nanocomposite blend GPE. The room temperature ionic conductivity of the gel electrolyte has been measured with different silica concentrations. The maximum ionic conductivity at room temperature has been observed as 4.3?×?10?3?S?cm?1 with 2 wt.% of SiO2 dispersion. The temperature dependence of ionic conductivity shows a typical Vogel-Tamman-Fulcher (VTF) behavior. The electrochemical potential window of the nanocomposite GPE film has been observed between ?1.6 V and 1.6 V. The optimized composition of the gel electrolyte has been used to fabricate a proton battery with Zn/ZnSO4·7H2O anode and PbO2/V2O5 cathode. The open circuit voltage (OCV) of the battery has been obtained as 1.55 V. The highest energy density of the cell has been obtained as 6.11 Wh?kg?1 for low current drain. The battery shows rechargeability up to 3 cycles and thereafter, its discharge capacity fades away substantially. 相似文献
10.
Jasneet Kaur N. S. Negi R. K. Kotnala Kuldeep Chand Verma 《Journal of Sol-Gel Science and Technology》2013,65(3):411-419
We have studied the effect of hydrothermal conditions at constant temperature of 180 °C, varying preparation time for 15, 30 and 45 h on nanostructures of diluted magnetic semiconductor Sn0.95Co0.05O2 (SC5). X-ray diffraction pattern confirm the tetragonal SnO2 rutile phase. The transmission and scanning electron microscopy shows the resulting nanostructures i.e. nanospheres and nanorods. The proposed reaction mechanism is given. The Raman spectra show the formation of tetragonal rutile structure of SC5 nanostructures. Fourier transform infrared spectrum has been used to verify the existence of Sn–O bond. The photoluminescence spectra show that the emission spectral intensity increases gradually with decreasing grains size, increasing hydrothermal heating time of SC5 samples and exhibits an intense blue luminescence centered at a wavelength of 531 nm. The optical absorbance measurements revealed that the nanometric size of the materials influences the energy band gap. All the prepared SC5 samples exhibit room temperature ferromagnetism. 相似文献