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New Extractive Spectrophotometric Method Development and Validation for the Estimation of Danazol in Pharmaceutical Formulations 萃取分光光度法测定复方丹那唑含量的新方法的建立与验证
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P169
K. Devi, K. Kumar, G. Krishnaveni
A simple, sensitive, selective, accurate and economical spectrophoto-metric method have been described in the present work for the deter-mination of danazol in bulk drug and pharmaceutical formulations (tablets). Method is based on the formation of yellow coloured ion-association complexes between danazol and alizarine red S in acid medium followed by their extraction with chloroform, exhibiting absorption maxima at 430 nm, and obeying Beer′s law in the concen-tration range of 5-30 μg/mL. Statistical analysis of the results of the proposed methods reveals high accuracy and good precision. The proposed methods could be successfully extended to the commercial pharmaceutical formulations containing danazol.
本文介绍了一种简便、灵敏、选择性好、准确、经济的测定原料药和制剂(片剂)中那那唑的分光光度法。该方法是利用那那唑和葱红S在酸性介质中形成黄色离子缔合物,然后用氯仿提取,在430 nm处出现最大吸收,在5 ~ 30 μg/mL浓度范围内符合比尔定律。统计分析结果表明,所提出的方法具有较高的准确度和精密度。所提出的方法可以成功地扩展到含有那那唑的商业药物制剂。
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引用次数: 0
Antimicrobial Evaluation and Efficient Green Synthesis of 8-Substituted-2,5-dihydro-1,5-benzothiazepine Derivatives 8-取代-2,5-二氢-1,5-苯并噻唑类衍生物的抗菌评价及高效绿色合成
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P168
P. Sharma
8-Substituted-2,5-dihydro-1,5-benzothiazepine derivatives have been synthesized by the reaction of 1-(2-furyl)-3-(3,4-dimethoxyphenyl)-2-propenone with six 5-substiuted-2-minobenzenethiols in dry ethanol saturated with dry HCl gas and also in the presence of aluminium nitrate as catalyst in dry ethanol. All the newly synthesized compounds were characterized by analytical and spectral data comprising IR, 1H NMR, 13C NMR, 19F NMR and mass studies. All these compounds have also been evaluated for their antimicrobial assay against the Gram-positive bacteria, Staphylococcus aureus and the Gram-negative bacteria, Pseudomonas aeruginosa and the fungus, Candida albicans. The antifungal activity was found to be more significant than antibacterial activity.
以6个5-取代-2-氨基苯乙醇与1-(2-呋喃基)-3-(3,4-二甲氧基苯基)-2-丙烯为原料,在干燥乙醇中以干HCl气体饱和和硝酸铝为催化剂的条件下,合成了8-取代-2,5-二氢-1,5-苯并噻吩衍生物。所有新合成的化合物都通过IR, 1H NMR, 13C NMR, 19F NMR和质量研究等分析和光谱数据进行了表征。所有这些化合物还对革兰氏阳性菌金黄色葡萄球菌和革兰氏阴性菌铜绿假单胞菌和真菌白色念珠菌进行了抗菌试验评价。抗真菌活性比抗菌活性更显著。
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引用次数: 0
Microwave-Assisted Synthesis and Anti-inflammatory Activity Evaluation of α-Aminophosphonates α-氨基膦酸盐的微波合成及抗炎活性评价
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P164
B. Sujatha, P. Kamala
In the present report, an expeditious green synthetic approach was developed for the synthesis of α-aminophosphonates 5(a-j) in good yields through one-pot three component reaction (Kabachnik-Fields reaction) in solvent-free conditions under microwave irradiation. The newly synthesized compounds were characterized by IR, NMR (1H, 13C and 31P), mass and C, H, N analysis. The synthesized compounds were screened for their anti-inflammatory activity using rat paw edema method. Most of the compounds from the series showed significant (p < 0.05) anti-inflammatory activity.
本文研究了一种在无溶剂条件下微波辐照下,通过一锅三组分反应(Kabachnik-Fields反应)快速合成α-氨基膦酸盐5(a-j)的绿色合成方法。通过IR、NMR (1H、13C和31P)、质量和C、H、N分析对新合成的化合物进行了表征。采用大鼠足跖水肿法对合成的化合物进行抗炎活性筛选。大部分化合物具有显著的抗炎活性(p < 0.05)。
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引用次数: 0
A Novel Stability Indicating RP-HPLC Method Development and Validation for Simultaneous Estimation of Bictegravir, Emtricitabine and Tenofovir in Pure and Fixed Dose Combination 一种新的稳定性指示反相高效液相色谱法同时测定比替格拉韦、恩曲他滨和替诺福韦的纯和固定剂量组合
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P163
G. Singh, T. Divakar
A novel, simple, precise, accurate stability indicating liquid chromato-graphy method was developed for the separation and simultaneous quantification of bictegravir, emtricitabine, tenofovir in bulk drug and pharmaceutical formulations. Separation was achieved on ProntoSILHypersorb ODS C18 column using mobile phase of 0.1 M sodium perchlorate, methanol in the ratio of 65:35 (v/v), pH 4.8 at a flow rate of 1.0 mL/min and UV detection was monitored at a wavelength of 258 nm. In these conditions, well resolved peaks were observed with acceptable system suitability at a retention time of 4.6 min for bictegravir, 7.0 min for emtricitabine and 10.1 min for tenofovir. Very high correlated linearity range was found to be 5-30 μg/mL for bictegravir, 20-120 μg/mL for emtricitabine and 2.5-15 μg/mL for tenofovir. The method can separate and identify the unknown degradation compounds formed during stress degradation study.
建立了一种简便、精确、准确、稳定的指示型液相色谱法,用于原料药和制剂中比替格拉韦、恩曲他滨、替诺福韦的分离和同时定量。采用prontosilhyperorb ODS C18色谱柱进行分离,流动相为0.1 M高氯酸钠,甲醇比为65:35 (v/v), pH为4.8,流速为1.0 mL/min,波长为258 nm。在这些条件下,在比替重力韦、恩曲他滨和替诺福韦的保留时间分别为4.6 min、7.0 min和10.1 min的情况下,观察到良好的分离峰,并具有可接受的系统适用性。比替替韦在5 ~ 30 μg/mL、恩曲他滨在20 ~ 120 μg/mL、替诺福韦在2.5 ~ 15 μg/mL范围内呈极好的线性相关。该方法可以分离和鉴定应力降解研究过程中形成的未知降解化合物。
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引用次数: 1
Microwave Mediated Michaelis-Arbuzov Reaction to Synthesize Bioactive Phenylphosphonate Derivatives Under Solvent Free Condition 无溶剂条件下微波介导Michaelis-Arbuzov反应合成生物活性苯膦酸盐衍生物
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P162
B. Sujatha, C. Subramanyam, K. P. Rao
Microwave assisted easy, efficient, and environment friendly process has been devised for the synthesis of phosphonates within minutes via microwave-assisted Michaelis-Arbuzov reaction. The desired products were obtained in excellent yields and in high purity under solvent-free and catalyst-free conditions. The structure of all the synthesized compounds was confirmed by spectral and CHN analysis. in vitro Antibacterial and antifungal activity of these compounds was also analyzed. Majority of the title compounds showed good inhibition towards bacteria and fungi.
利用微波辅助Michaelis-Arbuzov反应,设计了一种简单、高效、环保的合成膦酸盐的工艺。在无溶剂和无催化剂的条件下,得到了收率高、纯度高的理想产物。所有化合物的结构均通过光谱和CHN分析得到证实。并对这些化合物的体外抗菌和抗真菌活性进行了分析。大多数标题化合物对细菌和真菌有良好的抑制作用。
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引用次数: 2
Synthesis, Characterization and Anti-inflammatory Activity of New Pyrimidines 新型嘧啶的合成、表征及抗炎活性研究
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P178
P. Priyadarsini, V. Rao, C. Rao
The synthesis of some pyrimidine derivatives was achieved by conden-sation of 2-hydroxyacetophenone and cinnamic acid as starting materials through 1,3-diketones as intermediates. The resulting diketones have been converted into substituted pyrimidines by reaction with urea, thiourea and guanidine in the presence of trace of triethylamine and pyridine in calculated quantity. The synthesized compounds were characterized by their physical properties, NMR and LC-mass spectroscopic studies and also screened for their anti-inflammatory activity.
以2-羟基苯乙酮和肉桂酸为原料,以1,3-二酮为中间体缩合合成了一些嘧啶衍生物。在计算量的微量三乙胺和吡啶存在下,与尿素、硫脲和胍反应生成取代嘧啶。对合成的化合物进行了物理性质、核磁共振、质谱等表征,并对其抗炎活性进行了筛选。
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引用次数: 0
Bio-analytical Development and Validation of RP-HPLC Liquid Method for Quantification of Dapagliflozin Propanediol in Spiked Human Plasma RP-HPLC液相法定量人血浆中达格列净丙二醇的生物分析方法建立与验证
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P167
P. Subbareddy, T. Divakar
The purpose of the present research was to develop a suitable simple and reproducible RP-HPLC method for a quantification of dapagliflozin propanediol in spiked human plasma samples. The liquidliquid extraction plasma spiked samples of dapagliflozin propanediol were analyzed by using a ODS C18 Prontosil column under isocratic conditions. The extracted plasma spiked samples were carried using methanol, acetonitrile and pH 5.6 acetate buffer in the ratio of 50:20:10 (v/v) with a flow rate of 0.9 mL/min. The detector response was monitored at 228 nm using UV detector. The method was validated as per the ICH guidelines for bio analytical method validation and all the validation parameterswere found to be within the acceptance limit The plasma spiked samples shows stability at room temperature over a period of 48 h. Thus, this method would be employed for routine quantification of dapagliflozin in human plasma samples.
本研究的目的是建立一种简便、重现性好的反相高效液相色谱法定量人血浆中达格列净丙二醇的含量。采用ODS C18型Prontosil色谱柱,在等压条件下对达格列净丙二醇的液液萃取血浆加标样品进行了分析。提取的血浆加标样品用甲醇、乙腈和pH 5.6的醋酸缓冲液以50:20:10 (v/v)的比例携带,流速为0.9 mL/min。在228 nm处用紫外检测器监测探测器的响应。该方法按照ICH生物分析方法验证指南进行了验证,所有验证参数均在可接受范围内。血浆加标样品在室温下48小时内表现出稳定性。因此,该方法可用于人血浆样品中达格列净的常规定量。
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引用次数: 0
Seasonal Variation of Essential Oils Composition of A Medicinal Plant - Ocimum sanctum (Purple) 药用植物紫檀精油成分的季节变化
Pub Date : 2019-03-30 DOI: 10.14233/AJOMC.2019.AJOMC-P165
M. Rama, B. S. Sundar
The present study deals with the extraction of total essential oils from medicinal plant Ocimum sanctum (Purple) in four different seasons of 2010 calendar year. Extraction of total essential oil content of plant materials was carried out by Soxhlet extraction whereas extraction of volatile oils by steam distillation using Clevenger type apparatus. Total essential oil and volatile oils are more in winter season (November month) whereas very less quantity in summer season (May month). Eugenol is the major constituent present in the plant. The percentage composition of eugenol in four seasons was found from gas chromatography analysis.
本研究对药用植物紫荆(Ocimum sanctum,紫色)在2010年四个季节的总精油提取进行了研究。植物总挥发油的提取采用索氏提取法,挥发油的提取采用蒸汽蒸馏法。总精油和挥发油在冬季(11月)较多,而在夏季(5月)较少。丁香酚是这种植物的主要成分。气相色谱法测定了四季丁香酚的百分比组成。
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引用次数: 0
Rational Lead Optimization Based on the Modeled Structure ofCysteine Protease of Leishmania donovani 基于多诺瓦利什曼原虫半胱氨酸蛋白酶模型结构的合理导联优化
Pub Date : 2019-01-01 DOI: 10.14233/ajomc.2019.ajomc-p239
M. Patra
In present study, the molecular modeling techniques were applied to generate a refined model of a cysteine protease of Leishmania donovani using the crystal structure of a homologous protease and used for lead optimization. The structures of a series of complexes of the protease with the designed inhibitors were predicted using a novel docking technique comprising of repeated cycles of molecular dynamics and energy minimization. Calculation of the free energies of binding of the model with the designed inhibitors suggested that three compounds can form stable complexes with dissociation constants in the nanomolar range (0.038-1.41 nM). Search in the human genome revealed that a number of proteases of the cathepsin family had high homology with the parasite protease with amino acid identity around 45 %. The X-ray structures of all these were available in the protein data bank. The structures of the complexes of the selected inhibitors with a few homologous human proteases of known 3-D structures were also predicted using the same technique of optimization. The electrostatic potentials around the binding sites of the proteases were highly negative, which served as a clue for the introduction of positively charged groups in the designed inhibitors for higher affinity. The comparison of interaction energies and hydrogen bonding patterns among these complexes and similar complexes with homologous human proteases allowed us to short-listed three molecules as effective antileishmanial cysteine protease inhibitors.
本研究采用分子模拟技术,利用多诺瓦利什曼原虫半胱氨酸蛋白酶的晶体结构,建立了多诺瓦利什曼原虫半胱氨酸蛋白酶的精细模型,并用于铅优化。利用分子动力学的重复循环和能量最小化的新对接技术,预测了蛋白酶与所设计抑制剂的一系列配合物的结构。模型与所设计抑制剂的结合自由能计算表明,三种化合物可以形成稳定的配合物,解离常数在纳摩尔范围内(0.038 ~ 1.41 nM)。在人类基因组中搜索发现,组织蛋白酶家族的许多蛋白酶与寄生虫蛋白酶具有高度的同源性,氨基酸同源性约为45%。所有这些蛋白的x射线结构都可以在蛋白质数据库中找到。利用相同的优化技术预测了所选抑制剂与几种已知三维结构的同源人蛋白酶的配合物结构。蛋白酶结合位点周围的静电电位为高度负的,这为在设计的抑制剂中引入带正电的基团提供了线索,以获得更高的亲和力。通过比较这些配合物和类似配合物与同源人蛋白酶之间的相互作用能和氢键模式,我们筛选出了三种有效的抗利什曼半胱氨酸蛋白酶抑制剂。
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引用次数: 0
Synthesis, Characterization and Biological Evaluation of Ethyl-4'-(cyclopropanecarboxamido-N-yl)-5-ary-3-oxo-3,4,5,6-tetrahydro-biphenyl-4-carboxylate 4′-(环丙烷羧基氨基- n -基)-5-ary-3-氧-3,4,5,6-四氢联苯-4-羧酸乙酯的合成、表征及生物学评价
Pub Date : 2019-01-01 DOI: 10.14233/ajomc.2019.ajomc-p196
P. Akbari, V. Shah
A series of new substituted cyclohexenone derivatives have been synthesized by the reaction of various substituted chalcones with ethylacetoacetate. Some new N-(4-(3-aryl-acryloyl)phenyl)cyclopropane carboxamide were prepared by Claisen-Schmidt condensation method in presence of sodium hydroxide in ethanol solvent under stirring. The synthesized compounds were characterized by their spectral (IR, NMR, Mass) data and screened for their antimicrobial activities against Gram-positive and Gram-negative bacteria by using standard antimicrobial drugs.
以各种取代查尔酮与乙酰乙酸乙酯为原料,合成了一系列新的取代环己酮衍生物。采用Claisen-Schmidt缩合法制备了N-(4-(3-芳基-丙烯基)苯基)环丙烷甲酰胺。采用红外光谱、核磁共振光谱、质谱等方法对合成的化合物进行了表征,并采用标准抗菌药物对其抑菌活性进行了筛选。
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引用次数: 0
期刊
Asian Journal of Organic & Medicinal Chemistry
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