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Synthesis, Characterize and Evaluation of anti-bacterial and anti-fungal activity of thiazines 噻嗪类化合物的合成、表征及抑菌活性评价
Pub Date : 2019-01-12 DOI: 10.33974/ijrpca.v1i1.26
Arsalan Sarmad, R. Sultana, B. Salman
1,3 – Thiazines have been applied as useful starting materials in the stereo selective synthesis of compounds of pharmacological interest and they have served as chiral ligants and auxiliaries in enantioselective transformation. The thiazines are of great importance because they act as precursor for the synthesis of Cephalosporins (3,6-dihydro-2H-,1,3-thiazine) and then converted to the thiazine derivatives (an heterocyclic compounds). Therefore, it was thought to combine chalcones moiety to thiazine derivative together in a molecular frame work to see the biological activities, additive effort of these rings towards biological activities like Anti- bacterial and Anti- fungal activities.
1,3 -噻嗪类化合物已被应用于立体选择性合成中,并在对映体选择性转化中作为手性配体和助剂。噻嗪具有重要意义,因为它们是合成头孢菌素(3,6-二氢- 2h - 1,3-噻嗪)的前体,然后转化为噻嗪衍生物(杂环化合物)。因此,人们认为将查尔酮部分与噻嗪衍生物结合在一个分子框架中,观察这些环的生物活性,以及它们对生物活性的加性作用,如抗细菌和抗真菌活性。
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引用次数: 2
Development and validation of new analytical method for the simultaneous estimation of ibuprofen and diphenhydramine in bulk and pharmaceutical dosage form by RP-HPLC 反相高效液相色谱法同时测定布洛芬和苯海拉明原料药和制剂含量的新方法的建立与验证
Pub Date : 2018-09-19 DOI: 10.33974/ijrpca.v1i1.16
Pavan Kumar, T. Supriya, B. Sivagami, R. Sireesha, R. C. Kumar, M. Babu
A simple, accurate, rapid and precise method was developed for the simultaneous estimation of Ibuprofen and Diphenhydramine in Pharmaceutical dosage form. Chromatogram was run through Inertsil ODS (250x4.6mm) 5µ. Mobile phase used was Acetonitrile and Phosphate buffer (45:55) at a flow rate of 1.0 ml/min and detection wavelength was found to be 260 nm. The retention time was found to be 2.32 min and 2.93 min for Ibuprofen and Diphenhydramine respectively. The accuracy and reliability of the method was assessed by evaluation of linearity, precision (intra-day and inter-day % RSD >2), accuracy (98-102%), specificity, LOD, LOQ values in accordance with ICH guidelines. The developed method is applicable for routine quality control analysis of selected combined dosage forms.
建立了一种简便、准确、快速、精密的同时测定药物剂型中布洛芬和苯海拉明含量的方法。色谱柱为Inertsil ODS (250x4.6mm) 5µ。流动相为乙腈-磷酸盐缓冲液(45:55),流速为1.0 ml/min,检测波长为260 nm。布洛芬和苯海拉明的保留时间分别为2.32 min和2.93 min。采用线性度、精密度(日内、日间% RSD >2)、准确度(98 ~ 102%)、专属性、LOD、LOQ值评价方法的准确性和可靠性。该方法适用于所选复方制剂的常规质量控制分析。
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引用次数: 1
Stability indicating RP-HPLC method development and validation for the simultaneous estimation of Grazoprevir and Elbasvir in bulk and pharmaceutical dosage form 稳定性指示RP-HPLC方法的建立和验证,用于同时估计Grazoprevir和Elbasvir的散装和药物剂型
Pub Date : 2018-07-11 DOI: 10.33974/ijrpca.v1i1.4
V. P. Kumar, A. Kumar, B. Sivagami, R. C. Kumar, M. Babu
A simple, Accurate and precise method was developed for the simultaneous estimation of the Grazoprevir and Elbasvir in Tablet dosage form. Chromatogram was run through Kromosil C18 (250 x 4.6 mm), 5m. Mobile phase containing Buffer: Acetonitrile taken in the ratio 45:55 was pumped through column at a flow rate of 1 ml/min. Buffer used in this method was Di Potassium Hydrogen ortho Phosphate. Temperature was maintained at 30°C. Optimized wavelength selected was 215 nm. Retention time of Elbasvir and Grazoprevir and were found to be 2.503 min and 3.004. %RSD of the Elbasvir and Grazoprevir were and found to be 0.3 and 0.4 respectively. %Recovery was obtained as 98.17% and 99.83% for Grazoprevir and Elbasvir respectively. LOD, LOQ values obtained from regression equations of Grazoprevir and Elbasvir were 0.24, 0.73 and 0.06, 0.19 respectively. Retention times were decreased and run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.
建立了Grazoprevir和Elbasvir片剂同时测定的简便、准确、精确的方法。色谱通过Kromosil C18 (250 × 4.6 mm), 5m。流动相含缓冲液:以45:55的比例取乙腈,以1ml /min的流速泵入柱中。本方法使用的缓冲液为磷酸二氢钾。温度保持在30°C。优选波长为215 nm。Elbasvir和Grazoprevir的滞留时间分别为2.503 min和3.004 min。Elbasvir和Grazoprevir的RSD分别为0.3和0.4。Grazoprevir和Elbasvir的回收率分别为98.17%和99.83%。回归方程得出Grazoprevir和Elbasvir的LOD、LOQ分别为0.24、0.73和0.06、0.19。该方法减少了滞留时间,缩短了运行时间,简便、经济,可用于工业中常规的质量控制试验。
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引用次数: 3
Method development and method validation of guaifenesin and dextromethorphan by RP-HPLC 用反相高效液相色谱法建立愈创甘油醚和右美沙芬的方法及方法验证
Pub Date : 2018-06-30 DOI: 10.33974/ijrpca.v1i1.25
P. Salomi, D. Nayak, T. Vimalakannan, K. Reddy
A new, simple, precise, accurate and reproducible RP-HPLC method for Simultaneous estimation of bulk and pharmaceutical formulations. Separation of Guaifenesin and Dextromethorphan was successfully achieve THERMO, C18, 250X4.6mm, 5µm or equivalent in an isocratic mode utilizing 0.1M KH2PO4: Methanol (60:40) at a flow rate of 1.0ml/min and eluate was monitored at 280nm, with a retention time of 3.259 and 4.164 minutes for Guaifenesin and Dextromethorphan respectively. The method was validated and there response was found to be linear in the drug concentration range of 50µg/ml to150 µg/ml for Guaifenesin and 50µg/ml to150 µg/ml for Dextromethorphan. The values of the correlation coefficient were found to 0.999 for Guaifenesin and 1for Dextromethorphan. respectively. The LOD and LOQ for Guaifenesin were found to be 0.597 and 1.991 respectively. The LOD and LOQ for Dextromethorphan were found to be 0.1072 and 0.3572 respectively. This method was found to be good percentage recovery for were found to be 99 and 100 respectively indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample so, the method specifically determines the analyte in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness.
一种简便、精确、准确、重现性好的反相高效液相色谱同时测定原料药和制剂含量的新方法。采用0.1M KH2PO4:甲醇(60:40),流速为1.0ml/min, THERMO, C18, 250X4.6mm, 5µm或等量分离,洗脱液在280nm处监测,愈创木酚和右美沙芬的保留时间分别为3.259和4.164分钟。结果表明:愈创甘油醚在50µg/ml ~ 150µg/ml范围内、右美沙芬在50µg/ml ~ 150µg/ml范围内呈线性关系;愈创甘油醚和右美沙芬的相关系数分别为0.999和1。分别。愈创木酚素的LOD和LOQ分别为0.597和1.991。右美沙芬的定量限和定量限分别为0.1072和0.3572。该方法的回收率分别为99和100,表明该方法具有较高的准确度。该方法的特异性表明,标准品的保留时间与样品的保留时间具有良好的相关性,因此,该方法可以在不受片剂剂型辅料干扰的情况下,对样品中的分析物进行特异性测定。根据ICH指南对该方法进行了线性、准确度、精密度、特异性和鲁棒性的广泛验证。
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引用次数: 0
RP-HPLC method development and validation for the estimation of antifungal drug terbinafine HCL in bulk and pharmaceutical dosage form 反相高效液相色谱法测定抗真菌药物特比萘芬HCL原料药和制剂剂型的含量及验证
Pub Date : 2018-06-30 DOI: 10.33974/ijrpca.v1i1.8
R. Sireesha, P Syam Vijayakar, V. P. Kumar, B. Sivagami, P. Sikdar, M. Babu
In the present work RP-HPLC method has been developed for the quantitative estimation of Terbinafine hydrochloride in bulk drug and pharmaceutical formulations. A rapid and sensitive RP-HPLC Method with PDA detection (220 nm) for routine analysis of in Bulk drug and Pharmaceutical formulation was developed. Chromatography was performed with mobile phase containing a mixture of Potassium dihydrogen phosphate and Acetonitrile (65:35 v/v) with flow rate 1.5 ml/min. The linearity was found to be in the range of 50-150 µg/ml with (r2=0.999). The proposed method was validated by determining sensitivity, accuracy, precision, LOD, LOQ and system suitability parameters according to ICH guidrelines.
建立了反相高效液相色谱法定量测定原料药和制剂中盐酸特比萘芬的含量。建立了一种快速、灵敏的PDA (220 nm)反相高效液相色谱(RP-HPLC)方法,用于原料药和制剂的常规分析。流动相为磷酸二氢钾与乙腈的混合物(65:35 v/v),流速为1.5 ml/min。在50 ~ 150µg/ml范围内呈线性关系(r2=0.999)。根据ICH指南,通过测定灵敏度、准确度、精密度、定量限、定量限和系统适用性参数,对该方法进行了验证。
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引用次数: 0
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International Journal of Research In Pharmaceutical Chemistry and Analysis
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