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Validated Spectrophotometric Assay of Cefepime Hydrochloride and Cefuroxime Sodium Using a Tetrazolium Salt 盐酸头孢吡肟和头孢呋辛钠的四唑盐分光光度法测定
Pub Date : 2012-01-01 DOI: 10.1155/2012/959624
M. El-Azazy, A. Shalaby
A simple, rapid and sensitive spectrophotometric method for the determination of micro amounts of cefepime hydrochloride and cefuroxime sodium is described. The method is based on reduction of 2,3,5-triphenyltetrazolium chloride (TTC) by the cited drugs in slightly alkaline medium leading to formation of a highly colored formazan derivative. Different variables affecting the color development were investigated and optimized. Absorbance measurements were made at 483 nm. Under the proposed conditions, this method is applicable over concentration range of 4–50 µg ml-1 with molar absorpitivities ranging from 5.208 x 103–1.217 x 104 L.mol-1.cm-1 and Sandell's sensitivities ranging from 1.007 x 10-3–2.727 x10-3 µg cm-2. The proposed method was successfully applied for analysis of the cited drugs in formulations and the recovery percentages ranged from 99.47 to 99.8%. The results obtained demonstrated that the proposed method is equally accurate, precise and reproducible as the reported methods thus it is recommended for quality control and routine analysis where time, cost effectiveness and high specificity of analytical techniques are of great importance.
建立了一种简单、快速、灵敏的分光光度法测定盐酸头孢吡肟和头孢呋辛钠微量含量的方法。该方法是基于引用的药物在微碱性介质中还原2,3,5-三苯基四氮唑氯(TTC),从而形成高度着色的甲酸衍生物。对影响显色性的不同因素进行了研究和优化。在483 nm处测定吸光度。在此条件下,该方法适用于浓度范围为4-50µg ml-1,摩尔吸光度范围为5.208 × 103-1.217 × 104 l mol-1。桑德尔的灵敏度范围为1.007 × 10-3-2.727 × 10-3µg cm-2。该方法成功地应用于制剂中被引药物的分析,回收率为99.47 ~ 99.8%。结果表明,所提出的方法与报道的方法同样准确、精确和可重复性,因此建议用于质量控制和常规分析,其中时间、成本效益和分析技术的高特异性非常重要。
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引用次数: 7
Efficient Production Process for Food Grade Acetic Acid by Acetobacter aceti in Shake Flask and in Bioreactor Cultures 醋酸杆菌摇瓶和生物反应器高效生产食品级醋酸的工艺研究
Pub Date : 2012-01-01 DOI: 10.1155/2012/965432
H. Awad, Richard Díaz, R. Malek, N. Othman, R. Aziz, H. E. Enshasy
Acetic acid is one of the important weak acids which had long history in chemical industries. This weak organic acid has been widely used as one of the key intermediate for many chemical, detergent, wood and food industries. The production of this acid is mainly carried out using submerged fermentation system and the standard strain Acetobacter aceti. In the present work, six different media were chosen from the literatures and tested for acetic acid production. The highest acetic acid production was produced in medium composed of glucose, yeast extract and peptone. The composition of this medium was optimized by changing the concentration of medium components. The optimized medium was composed of (g/L): glucose, 100; yeast extract, 12 and peptone 5 and yielded 53 g/L acetic acid in shake flask after 144 h fermentation. Further optimization in the production process was achieved by transferring the process to semi-industrial scale 16-L stirred tank bioreactor and cultivation under controlled pH condition. Under fully aerobic conditions, the production of acetic acid reached maximal concentration of about 76 g/L and 51 g/L for uncontrolled and controlled pH cultures, respectively.
醋酸是一种重要的弱酸,在化学工业中有着悠久的历史。这种弱有机酸已被广泛用作许多化工、洗涤剂、木材和食品工业的关键中间体之一。该酸的生产主要采用浸没发酵系统和标准菌株醋酸杆菌进行。在本工作中,从文献中选择了六种不同的培养基,并进行了乙酸生产试验。在葡萄糖、酵母浸膏和蛋白胨组成的培养基中,乙酸的产量最高。通过改变培养基组分的浓度,优化了该培养基的组成。优化培养基为(g/L):葡萄糖,100;酵母浸膏、12和蛋白胨5在摇瓶中发酵144 h,得到53 g/L的乙酸。通过将该工艺转移到半工业规模的16l搅拌槽生物反应器上,并在控制pH条件下进行培养,进一步优化了生产工艺。在完全好氧条件下,无控制pH和控制pH培养的乙酸产量分别达到76 g/L和51 g/L左右。
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引用次数: 19
Indirect Electrochemical Analysis of Crocin in Phytochemical Sample 植物化学样品中藏红花素的间接电化学分析
Pub Date : 2012-01-01 DOI: 10.1155/2012/967079
R. A. Dar, Pradeep Kumar Brahaman, S. Tiwari, K. S. Pitre
A new electroanalytical method has been developed for the quantitative determination of crocin in a sample of stigmas of saffron (Crocus sativus L.). Crocin is polarographically inactive. However, cysteine in 0.02 M NaCl, pH=5.2±0.01 produces a well defined wave/peak with E1/2/Ep= –0.47/–0.45 V vs. Ag/AgCl. On recording polarograms of a set of solution containing a fixed concentration of cysteine and varying concentrations of crocin under aforesaid experimental conditions a gradual decrease in peak height/diffusion current and a negative shift in peak potential was observed. Thus, indicating cysteine-crocin interaction. Amperometric titration indicated crocin to cysteine ratio of 1:2. The above amperometric titration procedure has been used to determine the concentration of crocin in a sample of saffron. Crystallization process was carried out for the extraction of crocin from dried powder of saffron stigmas. The crystallized crocin was identified by UV-Visible spectrophotometry(at 255 nm and 442 nm) and the quantitative analysis by the developed amperometric method. The concentration of crocin in saffron was found to be 2.13% and purity of isolated crocin 96.81%. The percent recovery varied from 98.56–100.31% and RSD (n=5) of 2.17%.The validation of the proposed procedure for the quantitative assay of crocin was examined via an evaluation of the repeatability, recovery, selectivity and relative standard deviation.
建立了藏红花柱头中藏红花素的电分析法。藏红花素在极谱上无活性。然而,半胱氨酸在0.02 M NaCl, pH=5.2±0.01条件下,与Ag/AgCl相比,E1/2/Ep= -0.47 / -0.45 V,产生清晰的波/峰。在上述实验条件下,记录一组含有固定浓度半胱氨酸和不同浓度藏红花素的溶液的极谱图,观察到峰高/扩散电流逐渐降低,峰电位呈负移动。因此,表明半胱氨酸-藏红花素相互作用。电流滴定显示藏红花素与半胱氨酸的比例为1:2。上述安培滴定法已用于测定藏红花样品中藏红花素的浓度。采用结晶法从藏红花柱头干粉中提取藏红花素。采用紫外可见分光光度法(255 nm和442 nm)对结晶的藏红花素进行了鉴定,并采用建立的安培法进行了定量分析。藏红花中藏红花素的含量为2.13%,藏红花素的纯度为96.81%。回收率为98.56 ~ 100.31%,RSD (n=5)为2.17%。通过对重复性、回收率、选择性和相对标准偏差的评价,验证了藏红花素定量分析方法的有效性。
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引用次数: 7
Staminate Flower of Cocos Nucifera as Green Inhibitor for Mild Steel in HCl Medium 在HCl介质中对低碳钢的抑绿作用
Pub Date : 2012-01-01 DOI: 10.1155/2012/138463
R. Rajalakshmi, A. Safina
Corrosion control methods, especially the use of inhibitors, have gained monumental importance in the present scenario of expunging corrosion and the quest for eco-friendly reasons continues. To arrive at an inexpensive non-toxic, eco-friendly inhibitor formulations the present study on the use of Staminate Flower extract of Cocos Nucifera has been carried out by the classical weight loss measurements and electrochemical polarization measurements. The acid extract could bring out a maximum of 97.3% inhibition of mild steel corrosion in 1M HCl. Thermodynamic parameters of the corrosion process were calculated from temperature study. The adsorptive behaviour of Staminate Flower extract in acid solution may be approximated both by Langmuir and Temkin type isotherms. The results obtained by Tafel, Linear polarization resistance, and impedance spectroscopy have been correlated with the classical weight loss measurements. Values of Tafel constant ba and bc confirmed that the Staminate Flower extract acts like mixed type inhibitor. Examination of the surface of the metal in the presence of the inhibitor confirmed the deposition of inhibitor on the metal surface. The Staminate Flower extract in HCl medium efficiently inhibits the corrosion and proved to be zero cost inhibitor, eco-friendly, non-toxic, and highly economical.
腐蚀控制方法,特别是抑制剂的使用,在消除腐蚀的当前情况下已经变得非常重要,对生态友好的追求仍在继续。为了获得一种廉价、无毒、环保的抑制剂配方,本文采用经典失重法和电化学极化法研究了椰子树雄蕊花提取物的使用。在1M HCl中,酸浸提液对低碳钢的缓蚀效果可达97.3%。通过温度研究计算了腐蚀过程的热力学参数。雄蕊花提取物在酸性溶液中的吸附行为可以用Langmuir等温线和Temkin等温线近似。用塔菲尔法、线性极化电阻法和阻抗谱法得到的结果与经典的失重测量结果相关联。Tafel常数ba和bc值证实了雄蕊花提取物具有混合型抑制剂的作用。在抑制剂存在的情况下对金属表面的检查证实了抑制剂在金属表面的沉积。在HCl介质中,Staminate Flower提取物能有效抑制腐蚀,是一种零成本、环保、无毒、经济的缓蚀剂。
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引用次数: 8
Melamine Trisulfonic Acid as a Highly Efficient and Reusable Catalyst for the Synthesis of β-Acetamido Ketones 三聚氰胺三磺酸作为合成β-乙酰胺酮的高效可重复使用催化剂
Pub Date : 2012-01-01 DOI: 10.1155/2012/173197
A. Zare
A highly efficient protocol for the one-pot multi-component condensation of acetophenones with aromatic aldehydes, acetonitrile and acetyl chloride in the presence of melamine trisulfonic acid (MTSA) as a highly efficient and recyclable sulfonic acid-containing catalyst at room temperature is described. In this method, β-acetamido ketone derivatives are obtained in high to excellent yields and in relatively short reaction times.
介绍了一种以三聚氰胺三磺酸(MTSA)为高效可回收的含磺酸催化剂,在室温下与芳醛、乙腈和乙酰氯进行一锅多组分缩合反应的高效方案。在这种方法中,β-乙酰氨基酮衍生物在相对较短的反应时间内以高至优异的收率得到。
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引用次数: 3
Development, Estimation and Validation of Lisinopril in Bulk and its Pharmaceutical Formulation by HPLC Method 赖诺普利原料药及其制剂的高效液相色谱法开发、评价与验证
Pub Date : 2012-01-01 DOI: 10.1155/2012/292754
V. B. Raju, A. Rao
An accurate and precise HPLC method was developed for the determination of lisinopril. Separation of the drug was achieved on a reverse phase C8 column using a mobile phase consisting of phosphate buffer and methanol in the ratio of 35:65v/v. The flow rate was 0.8 mL/min and the detection wavelength was 215 nm. The linearity was observed in the range of 20-60 μ g/mL with a correlation coefficient of 0.9992. The proposed method was validated for its linearity, accuracy, precision and robustness. This method can be employed for routine quality control analysis of lisinopril in tablet dosage forms.
建立了高效液相色谱法测定赖诺普利含量的方法。药物在反相C8柱上分离,流动相由磷酸盐缓冲液和甲醇组成,比例为35:65v/v。流速为0.8 mL/min,检测波长为215 nm。在20 ~ 60 μ g/mL范围内呈线性关系,相关系数为0.9992。该方法具有良好的线性度、准确度、精密度和鲁棒性。该方法可用于赖诺普利片剂的常规质量控制分析。
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引用次数: 7
New Spectrophotometric Method for the Determination of Bosentan - An Anti-Hypertensive Agent in Pharmaceutical Dosage Forms 分光光度法测定药物剂型中降压药波生坦含量的新方法
Pub Date : 2012-01-01 DOI: 10.1155/2012/359745
A. Narendra, D. Deepika, M. M. Annapurna
A new, simple and sensitive spectrophotometric method in ultraviolet region has been developed for the determination of Bosentan in bulk and in pharmaceutical formulations. Bosentan exhibits absorption maxima at 273 nm with apparent molar absorptivity of 1.3293×104 L/mol.cm in methanol and octane 1-sulfonic acid solvent mixture. Beer's law was found to be obeyed in the concentration range of 0.1-100 μg/mL. The method was validated as per the ICH guidelines.
建立了一种简便、灵敏的紫外分光光度法测定原料药和制剂中波生坦的含量。波生坦在273 nm处具有最大吸收,表观摩尔吸收率为1.3293×104 L/mol。Cm在甲醇和辛烷磺酸溶剂混合物中。在0.1 ~ 100 μg/mL浓度范围内符合Beer定律。该方法按照ICH指南进行了验证。
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引用次数: 5
Separation of m/p-Aminoacetophenone Using Hydrotropy 疏水法分离间/对氨基苯乙酮
Pub Date : 2012-01-01 DOI: 10.1155/2012/504767
M. Dhinakaran, Antony Bertie Morais, N. Gandhi
The aqueous solubilities of m/p-aminoacetophenone in different concentrations (0-3.0 mol/L) of hydrotropes such as diethyl nicotinamide, sodium pseudocumene sulfonate and sodium thiocyanate solutions at different system temperatures (303K to 333K) were studied. The percentage extraction (%E) of m- aminoacetophenone from m/p-aminoacetophenone mixture increases with increase in hydrotrope concentration. A Minimum Hydrotrope Concentration (MHC) in the aqueous phase was required to initiate the significance of the %E of m-aminoacetophenone. Percentage extraction (%E) is the ratio of moles of m-aminoacetophenone extracted in presence and absence of a hydrotrope. The sensitivity and feasibility of the proposed process are examined by carrying out solubilization and equilibrium precipitation experiments with the mixtures of various compositions. The effectiveness of hydrotropes was measured in terms of Setschenow constant Ks. The extraction data are also fitted in a polynomial equation as the function of hydrotrope concentration. The solubilized material can be recovered by dilution with water.
研究了m/对氨基苯乙酮在不同浓度(0 ~ 3.0 mol/L)的二乙基烟酰胺、伪文献烯磺酸钠和硫氰酸钠的水溶液中,在不同体系温度(303K ~ 333K)下的溶解度。对-氨基苯乙酮混合物中对-氨基苯乙酮的提取率(%E)随着水相浓度的增加而增加。对间氨基苯乙酮的%E的意义,需要在水相中有最小的水相浓度(MHC)。萃取百分数(%E)是在存在和不存在水同物的情况下萃取间氨基苯乙酮的摩尔数之比。通过对不同组分的混合物进行增溶和平衡沉淀实验,验证了该方法的敏感性和可行性。用Setschenow常数k来测量水的有效性。将提取数据拟合为含水化合物浓度的多项式方程。被溶解的物质可以用水稀释回收。
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引用次数: 5
Conductometric Study of Nimesulide in Aqueous Solutions of Hydrotropic Agents at Different Temperatures 不同温度下尼美舒利在亲水剂水溶液中的电导研究
Pub Date : 2012-01-01 DOI: 10.1155/2012/616943
Chandravir S. Solanki, P. Mishra, M. Talari, M. Tripathy, U. Dash
Conductance values of nimesulide have been determined in water in 0.1, 0.2, 0.4, 0.6, 0.8, 1 and 2 mol dm-3 aqueous solutions of hydrotropic agents (sodium benzoate, sodium salicylate, sodium bromide and nicotinamide) at temperatures 298.15, 303.15, 308.15 and 313.15 K. The conductance values have been used to evaluate the limiting molar conductance and association constants by means of Shedlovsky extrapolation technique. Thermodynamic parameters for the association process of nimesulide in aqueous solutions of hydrotropic agents have also been calculated.
在温度为298.15、303.15、308.15和313.15 K时,测定了尼美舒利在0.1、0.2、0.4、0.6、0.8、1和2 mol dm-3的亲水剂(苯甲酸钠、水杨酸钠、溴化钠和烟酰胺)水溶液中的电导值。利用谢德洛夫斯基外推法,用电导值来计算极限摩尔电导和缔合常数。计算了尼美舒利在亲水剂水溶液中缔合过程的热力学参数。
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引用次数: 13
Kinetic Determination of Paracetamol using a Novel Belousov-Zhabotinskii Oscillating System Catalyzed by a Tetraazamacrocyclic Complex 四氮杂环配合物催化的新型Belousov-Zhabotinskii振荡体系动力学测定扑热息痛
Pub Date : 2012-01-01 DOI: 10.1155/2012/626982
Hu Gang, Qin Wang, Min Meng, M. Lu, Fulin Zhao, Hu Lin
A new analytical method for determination of paracetamol is proposed. This method is based on a novel B-Z oscillating system, which involves a Tetraazamacrocyclic Complex [CuL](ClO4)2 as catalyst and malic acid as the substrate. The ligand L in the complex is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene. By perturbation mount of paracetamol on the B-Z system, there is a linear relationship between the changes in the oscillation amplitude and the logarithm of paracetamol concentration in the range 5×10-7 to 2×10-4 M, with a correlation coefficient of 0.99743. The effects of influential variables, such as the concentration of reaction components, temperature and on the determinations were studied. The probable mechanism involving the perturbation of paracetamol on the oscillating chemical system was also discussed.
提出了一种新的测定扑热息痛的分析方法。该方法基于一种新的B-Z振荡体系,该体系以四氮杂环配合物[CuL](ClO4)2为催化剂,苹果酸为底物。配合物中的配体L为5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四十四-4,11-二烯。通过对B-Z体系进行扑热息痛的扰动,在5×10-7 ~ 2×10-4 M范围内,振荡幅度的变化与扑热息痛浓度的对数呈线性关系,相关系数为0.99743。研究了反应组分浓度、反应温度等因素对测定结果的影响。讨论了扑热息痛对振荡化学体系的扰动的可能机理。
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引用次数: 3
期刊
E-journal of Chemistry
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