New method for the quantification of dequalinium cations in pharmaceutical samples by absorption and fluorescence diode array thin-layer chromatography

A diode array HPTLC method for dequalinium chloride in pharmaceutical preparations is presented. For separation a Nano TLC silica gel plate (Merck) is used with the mobile phase methanol—7.8% aqueous NH₄⁺CH₃COO⁻ (17:3, v/v) over a distance of 6 cm. Dequalinium chloride shows an R_F value of 0.58. Pure dequalinium chloride is measured in the wavelength range from 200 to 500 nm and shows several by-products, contour plot visualized in absorption, fluorescence and using the Kubelka–Munk transformation. Scanning of a single track in absorption and fluorescence measuring 600 spectra in the range from 200 to 1100 nm takes 30 s. As a sample pre-treatment of an ointment it is simply dissolved in methanol and can be quantified in absorption from 315 to 340 nm. The same separation can also be quantified using fluorescence spectrometry in the range from 355 to 370 nm. A new staining method for dequalinium chloride, using sodium tetraphenyl borate/HCl in water allows a fluorescence quantification in the range from 445 to 485 nm. The linearity range of absorption and fluorescence measurements is from 10 to 2000 ng. Sugar-containing preparations like liquids or lozenges with a reduced sample pre-treatment can be reliably quantified only in fluorescence. The total for the quantification of an ointment sample (measuring four standards and five samples), including all sample pre-treatment steps takes less than 45 min!     

Frequency-based views to pattern collections

Finding interesting patterns from data is one of the most important problems in data mining and it has been studied actively for more than a decade. However, it is still largely open problem which patterns are interesting and which are not.The problem of detecting the interesting patterns (in a predefined class of patterns) has been attempted to solve by determining quality values for potentially interesting patterns and deciding a pattern to be interesting if its quality value (i.e., the interestingness of the pattern) is higher than a given threshold value. Again, it is very difficult to find a threshold value and a way to determine the quality values such that the collection of patterns with quality values greater than the threshold value would contain almost all truly interesting patterns and only few uninteresting ones.To enable more accurate characterization of interesting patterns, use of constraints to further prune the pattern collection has been proposed. However, most of the constrained pattern discovery research has been focused on structural constraints for the pattern collections and the patterns. We take a complementary approach and focus on constraining the quality values of the patterns.We propose quality value simplifications as a complementary approach to structural constraints on patterns. As a special case of the quality value simplifications, we consider discretizing the quality values. We analyze the worst-case error of certain discretization functions and give efficient discretization algorithms minimizing several loss functions. In addition to that, we show that the discretizations of the quality values can be used to obtain small approximate condensed representations for collections of interesting patterns. We evaluate the proposed condensation approach experimentally using frequent itemsets.     

Colourimetric Determination of Pharmaceutical Thiocompounds and Allopurinol Using Mercurochrome

Abstract

A new, simple and sensitive colourimetric method for determination of three pharmaceutical thiocompounds: cimetidine, thiabendazole and carbimazole, and also allopurinol, has been presented. the method is based on the reaction of each drug with mercurochrome (MER) in aqueous alkaline medium to give an intense red coloured chromogen. Optimization of the reaction conditions has been investigated. Obedience to Beer's law permitted the successful application of the proposed method for the assay of the investigated drugs in different dosage forms. Compared with the Pharmacopoeial methods, the proposed method gave equally accurate (t-test) and precise (F-test) results.     

Comparison of thermal and elastic properties of glassy racemic and enantiomorphic ibuprofen studied by Brillouin light scattering and modulated differential scanning calorimetry

The vitrification process of racemic RS- and enantiomorphic S-ibuprofen was studied by using Brillouin light scattering and modulated differential scanning calorimetry (DSC). The sound velocity and the attenuation coefficient of both compounds were determined for the first time in the glassy, supercooled liquid and liquid states. The sound velocity and the hypersonic damping were similar between the two ibuprofen pharmaceuticals over the whole investigated temperature range including glassy, supercooled liquid and liquid states. The thermal expansion coefficient of the RS-ibuprofen was smaller than that of the S-ibuprofen, which suggests that the intermolecular force of the former is slightly stronger than the latter. The thermal relaxation times derived from the modulated DSC were consistent with the dielectric relaxation times in both RS- and S-ibuprofens. The fragility index of S-ibuprofen just above the glass transition was determined to be 73, which was smaller compared to the value of RS-ibuprofen, 89. This difference in the fragility indicates that the decrease in the fragility of S-ibuprofen compared to the racemic one may improve its stability of the amorphous state below the glass transition temperature against crystallization.     

An overview of the applications of capillary electrophoresis to the analysis of pharmaceutical raw materials and excipients

Summary The use of capillary electrophoresis for the separation and quantitation of a range of pharmaceutical raw materials and excipients is reviewed. Capillary electrophoresis is shown to be a useful and versatile technique for a large number of applications. Features of the various methods include simplicity, detection of poor chromatophore species by extensive use of indirect UV detection or direct absorbance at low wavelengths, minimal operating costs and generation of high quality retrievable raw data. Specific novel examples described include separations of lactose, flavouring agents, inorganic salts, lecithin constituents, a range of organic acids, benzylalkonium chloride components, sodium lauryl sulphate, and the quality of input water. It is concluded that the versatility of CE will ensure that it is increasingly used in the analysis of pharmaceutical raw materials and excipients.     

数据挖掘过程中连续属性离散化新方法研究

在知识发现和机器学习领域里,许多数据挖掘方法如基于粗集的数据挖掘工具等需要使用离散的属性值,但实际观测到的大多是连续性属性数据,这对许多新型数据挖掘工具的研究带来了不便.本文针对以上问题,在综合分析目前连续属性离散化方法的基础上,提出了一种基于数据分布特征的连续属性离散化新方法,并用经典算例验证了此算法,实验结果表明该方法具有合理性和可行性.     

普物实验教学改革初探

本文叙述普物实验教学改革的几点做法及其效果。     

四苯硼钠沉淀／ICP－AES间接测定药物奎宁的研究

本文提出了以四苯钠为沉淀剂，ＩＣＰ－ＡＥＳ间接测定药物成份奎宁的新方法。对影响沉淀反应的条件进行了详细考察和优化，在选择好的实验条件下，本法的检出限为０．０７μｇ／ｍＬ，ＲＳＤ为４％。实验表明，较大量的基体（碱土金属Ｃａ和Ｍｇ）存在对测定结果无明显影响，但可与试剂反应的Ｋ＋、产生正干扰。本法已用于复方奎宁注射液中有效药物成份的测定，分析结果满意。