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131.
A method is proposed for the extraction and mutual separation of quadrivalent titanium, zirconium and hafnium from hydrochloric acid using triphenylphosphine oxide dissolved in toluene as an extractant. The optimum conditions for the extraction and separation have been evaluated from critical study of acid concentration, extractant concentration, period of equilibration and effect of diluent. The effect of foreign ions on the extraction and determination is also discussed. The probable composition of the extracted species has been deduced from logD-logC plots. The method affords mutual separation of titanium, zirconium and hafnium and is applicable to the analysis of alloy samples. 相似文献
132.
Silver compounds are used in pharmaceutical and ayurvedic medicines. A method is proposed for the extraction separation of silver from Cu, Cd, Zn, Ni, Pt (IV) and Au (III) from nitrate solution using triphenylphosphine sulphide as an extractant. The recovery of silver is tested both volumetrically and/or by ICP-AES technique. 相似文献
133.
The first total synthesis of (+)-1S-minwanenone, an archetypical seco-prezizaane sesquiterpene, has been accomplished from a readily available chiral endo-tricyclic synthon following a flexible strategy. 相似文献
134.
Kaul N Agrawal H Maske P Rao JR Mahadik KR Kadam SS 《Journal of separation science》2005,28(13):1566-1576
Two sensitive and reproducible methods are described for the quantitative determination of itopride hydrochloride (IH) in the presence of its degradation products. The first method is based on HPLC separation on a reversed phase Kromasil column [C18 (5-microm, 25 cm x 4.6 mm, ID)] at ambient temperature using a mobile phase consisting of methanol and water (70:30, v/v) adjusted to pH 4.0 with orthophosphoric acid with UV detection at 258 nm. The flow rate was 1.0 mL per min with an average operating pressure of 180 kg/cm2. The second method is based on HPTLC separation on silica gel 60 F254 using toluene:methanol:chloroform:10% ammonia (5.0:3.0:6.0:0.1, v/v/v/v) as mobile phase at 270 nm. The analysis of variance (ANOVA) and Student's t-test were applied to correlate the results of IH determination in dosage form by means of HPLC and HPTLC methods. The drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment, UV, and photodegradation. The proposed HPLC method was utilized to investigate the kinetics of the acidic, alkaline, and oxidative degradation processes at different temperatures and the apparent pseudo-first-order rate constant, half-life, and activation energy were calculated. In addition the pH-rate profile of degradation of IH in constant ionic strength buffer solutions in the pH range 2-11 was studied. 相似文献
135.
P. Madhavan B. M. Rao Pravin Abhishek P. R. Kumar M. Sreenivasulu K. B. Chandrasekhar 《Chromatographia》2007,65(1-2):81-84
A normal phase chiral LC method for chiral purity evaluation of β-amino-β-(4-methoxyphenyl) propionic acid was developed on
donor–acceptor (pirkle) column. The chiral stationary phase used was a 250 × 4.6 mm (R, R) Whelk-01 with 5 μm particle size,
which was accompanied with a 1 cm long guard column. The “hybrid” pi-electron donor–acceptor based stationary phase (R, R)
Whelk-01 was found to be enantiomeric selective for (R) and (S) enantiomers of β-amino-β-(4-methoxyphenyl) propionic acid
with a resolution >2.5. The concentration of 2-propanol and TFA in the mobile phase plays an important role on the chrmatographic
efficiency and resolution between the enantiomers. The limit of detection and limit of quantification of (S) enantiomer was
0.3 and 1.0 μg mL-1 for 20 μL injection volume. The percentage RSD of the peak area of six replicate injections of (S) enantiomer at LOQ concentration
was 4.5. The percentage recovery of (S) enantiomer from (R) enantiomer samples ranged from 92 to 100. The test solution was
observed to be stable up to 24 h after the preparation. The developed method was also checked by different analysts and on
different lots of columns, reagents and it was proved to be rugged. The developed normal phase chiral LC method can be used
for the determination of the enantiomeric purity of R-β-amino-β-(4-methoxyphenyl) propionic acid. 相似文献
136.
Complexes of ammonia with propane and cyclopropane: electrostatic guidelines for ab initio treatment
A model based on the molecular electrostatic potential (MESP) is employed for the investigation of structures and energies
of complexes of ammonia with propane and cyclopropane. The electrostatic model geometries are employed as starting points
for an ab initio investigation at the self-consistent field and second-order M?ller-Plesset (MP2) levels. The most stable
structures of C3H6..NH3 and C3H8..NH3 complexes have the interaction energies of 10.07 kJ/mol and 8.15 kJ/mol, respectively, at the MP2/6-31G(d,p) level. The energy rank order of the structures is not altered with the use of the 6-31++G(d,p) basis set, and the basis␣set superposition error has little effect. The interaction energy decomposition analysis shows
that the electrostatic component is dominant over the other ones. MESP topography thus seems to offer valuable hints for predicting
the structures of weakly bonded complexes.
Received: 8 July 1998 / Accepted: 4 August 1998 / Published online: 2 November 1998 相似文献
137.
A method is developed for extraction of gold(III) (75–300 g) from hydrochloric acid solution with triphenylarsine oxide dissolved in toluene as extradant. Gold(III) is determined spectrophotometrically with stannous chloride. The extraction is quantitative from 1.5–1.9M hydrochloric acid with 0.25% triphenylarsine oxide and an equilibration period of 30s. The method permits separation of gold(III) from Cu(II), Pt(IV), Pd(II), Ni(II), Zn(II), Cd(II) and Hg(II) and its spectrophotometric determination in ayurvedic medicines. The recovery and relative standard deviation obtained are >99.0% and <1.0%. 相似文献
138.
A simple, rapid, and precise method is developed for the quantitative simultaneous determination of metformin and pioglitazone in a combined pharmaceutical-dosage form. Separation is achieved with a Zorbax XDB C(18), 15-cm analytical column using buffer-acetonitrile (66:34, v/v) of pH 7.1, adjusted with orthophosphoric acid as the mobile phase. The buffer used in the mobile phase contains 10mM disodium hydrogen phosphate and 5mM sodium dodecyl sulphate in double-distilled water. The instrumental settings are flow rate of 1 mL/min, column temperature at 40 degrees C, and detector wavelength of 226 nm. The internal standard method is used for the quantitation of the ingredients of this combination. Methylparaben is used as an internal standard. The method is validated and shown to be linear for metformin and pioglitazone. The correlation coefficients for metformin and pioglitazone are 0.9991 and 0.9999, respectively. The relative standard deviations for six replicate measurements in two sets of each drug in the tablets are always less than 2%. 相似文献
139.
Ion-pair extraction and determination of copper(II) and zinc(II) in environmental and pharmaceutical samples. 总被引:1,自引:0,他引:1
Copper and zinc were extracted from salicylate solution into Aliquat 336 dissolved in toluene and determined in the organic phase spectrophotometrically using 1-(2-pyridylazo)-2-naphthol. The determination of copper and zinc was also carried out titrimetrically or by atomic absorption spectrometry after stripping the metal ions from the organic phase. The method permits the determination of copper and zinc in environmental and pharmaceutical samples. The standard deviation and relative standard deviation are 0.052 micrograms and 0.69%, respectively, for copper and 0.041 micrograms and 0.60%, respectively, for zinc. 相似文献
140.
In an approach towards the enantioselective total synthesis of the novel bioactive natural product Sch 642305, an unusual diastereoselection during the key RCM reaction, resulted in the synthesis of the 11-epi-isomer of Sch 642305. 相似文献