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11.
An experimental mixture design was applied to a differential scanning calorimetry (DSC) study performed to evaluate naproxen
compatibility in tablet formulations consisting of four classic excipients (sorbitol, sodium carboxymethylcellulose, poly(ethylene
glycol) 20000 and Veegum) each in adequate concentration ranges accounting for the relevant values actually used in pharmaceutical
formulations. Twenty-seven different tablets were obtained from as many mixtures prepared according to the experimental design
plan and analyzed in a random order by DSC. Statistical evaluation of experimental data enabled correlation of both enthalpy
and onset temperature variations of drug melting endotherm (selected as responses indicative of the presence of drug-excipient
interactions) with the mixture composition. Variance analysis (Anova) confirmed the reliability of the postulated polynomial
model in providing adequate prediction of true system behaviour.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
12.
A simple high-performance liquid chromatographic method – ion-pair reversed- phase high performance liquid chromatography (RPIC) has been developed and employed for the analysis of zoledronic acid and its related substances in bulk material and commercial dosage forms. The mobile phase was a mixture of methanol (20%) and 5 mmol L–1 phosphate buffer (80%) containing 6 mmol L–1 tetrabutylammonium bromide, adjusted to pH 7.0 with sodium hydroxide. C8 column was used as the stationary phase. The chromatographic conditions were optimized. The active ingredient – zoledronic acid was successfully separated from its related substances, including remained imidazol-1-yiacetic acid in the synthesis of zoledronic acid and other possible impurities of oxidation and decomposition. The excipients did not interfere with the determination of zoledronic acid in commercial dosage formulations. The method was rapid, simple, accurate and reproducible. It was not only successfully employed for the assay of zoledronic acid in bulk material and pharmaceutical dosage forms but also for the determination of its related substances. 相似文献
13.
ABSTRACTCo-crystallization frequently employs forces such as hydrogen bonds, halogen bonds, and π-π stacking to assemble molecules in a multi-component crystal. In an effort to increase the strength of the intermolecular interaction between the anti-cholesterol drug bezafibrate (BEZA), a wastewater contaminant, and hydrogen-bond-acceptor molecules, we modified the pKa values of the acceptors. Here, we describe the first series of salts incorporating BEZA and achieve a variety of supramolecular architectures including discrete assemblies, 1D chains, tapes, and 2D sheets. We discuss exceptions to the pKa rule, and demonstrate that the presence of hydrogen-bond-donor atoms on the acceptor molecule supports salt formation. 相似文献
14.
《Electroanalysis》2004,16(9):741-747
This work reports a technique for the rapid electrochemical detection of propranolol and metoprolol in pharmaceutical preparations using stabilized lipid films. Microporous filters composed of glass fibers (nominal pore sizes 0.7 and 1.0 μm) were used as supports for the formation and stabilization of these devices. The lipid film is formed on the filter by polymerization prior to its use. This stabilized after storage in air. Lipid films composed of phosphatidylcholine were used for the detection of propranolol and metoprolol in pharmaceutical preparations. The stabilized lipid membranes provided artificial ion gating events in the form of transient signals within about 60 and 34 s after exposure of the membranes to propranolol and metoprolol, respectively. The magnitude of the transient current signal was related to the concentration of propranolol and metoprolol in bulk solution in the micromolar range. The mechanism of signal generation was investigated by differential scanning calorimetric studies. These studies revealed that the adsorption of the drug is through the hydrophobic aryl terminal of the compound, whereas the hydrophilic groups were directed towards the electrolyte solution. This adsorption caused a rapid alteration of the electrochemical double layer of the lipid film (i.e., capacitance changes) that resulted in the transient ion current signal. The present technique was used for the rapid detection of propranolol and metoprolol in pharmaceutical preparations and can function for repetitive uses after storage in air. Future research is targeted to the determination of these chemicals in human biofluids such as urine of athletes. 相似文献
15.
双嘧达莫的荧光光谱分析法 总被引:9,自引:0,他引:9
以荧光光谱法研究了双嘧达莫在溴化十六烷基三甲基铵(CTMAB)、β_环糊精 (β_CD)、十二烷基硫酸钠 (SDS)等介质体系中的荧光性质 ,发现CTMAB、SDS和 β_CD对双嘧达莫均有不同程度的荧光增敏作用 ,提出了在CTMAB、SDS和 β_CD水溶液中测定双嘧达莫的荧光光谱分析法 ;该法灵敏度高 ,检出限低(3.20×10 -9mol/L) ,在6.40×10 -8~3.20×10 -6mol/L范围内荧光强度与双嘧达莫的浓度呈良好线性关系 相似文献
16.
Oxidative cyclization of 2-pyrrolidinyl-acetamide and 2-pyrrolidinyl-propionamide local anaesthetics
2 - Pyrrolidinyl - acetamide and -propionamide local anaesthetics (1a–d) on oxidation with mercuric acetate, potassium hexacyanoferrate(III) and potassium permanganate underwent oxidative cyclization to give new bicyclic compounds, hexahydro - 1H - pyrrolo[1,2 - a]imidazolin - 2 - ones (2a–d). The propionamides (1c–d) yielded mixtures of the two possible diastereoisomers of 2c and 2d. These were separated; in solution and above their melting points they epimerized via ring opening and reclosure between the 7a-carbon and 1-nitrogen atoms. 相似文献
17.
Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects.Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur.The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 m Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5.Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce. 相似文献
18.
The fluorimetric determination of adrenaline is carried out in a continuous-flow assembly and by means of the molecular dissolved oxygen. The sample solution merges with an NaOH stream, then the resulting mixture is heated at 73 °C and led to the flow-cell of the fluorimeter. The flow-assembly is very simple and the procedure is quick (107 samples h–1) reproducible (R.S.D. 0.6%), selective and suitable to be applied to determination of adrenaline in formulations. Calibrations graph are linear over the ranges 0.05–15 and 20–40 mgl–1. 相似文献
19.
Two vibrational spectrometry-based methodologies were developed for Metamitron determination in pesticide formulations. Fourier transform-middle infrared (FT-MIR) procedure was based on the extraction of Metamitron by CHCl3 and latter determination by peak area measurement between 1556 and 1533 cm−1, corrected with a two points baseline established from 1572 to 1514 cm−1. Fourier transform-near infrared (FT-NIR) determination was made after the extraction of Metamitron in acetonitrile and measuring the peak area between 6434 and 6394 cm−1 corrected using a two points baseline defined between 6555 and 6228 cm−1. Repeatability, as relative standard deviation, of 5 independent measurements at mg g−1 concentration level, of 0.16% and 0.07% for MIR and NIR and a limit of detection of 0.03 and 0.004 mg g−1 were obtained for MIR and NIR, respectively.NIR determination provides a sample frequency of 120 h−1, higher than that found by MIR and liquid chromatographic methods (60 and 15 h−1, respectively). On the other hand, the NIR method reduces the solvent consumption and waste generation, to only 1 ml acetonitrile per sample as compared with 3.4 ml chloroform required for the MIR determination and 60 ml acetonitrile used in the chromatographic reference procedure. So, vibrational procedures can be considered serious alternatives to long and time consuming chromatographic methods usually recommended for quality control of commercially available pesticide formulations. 相似文献
20.