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Validated Analytical Method for Multicomponent Analysis of Famotidine and Ofloxacin in Bulk drug and Tablet Formulation by using UV-Visible Spectrophotometer and RP-HPLC 验证了用紫外可见分光光度法和反相高效液相色谱法分析原料药和片剂中法莫替丁和氧氟沙星含量的方法
Pub Date : 2023-09-07 DOI: 10.52711/2231-5675.2023.00026
Pooja Kaushal, Shiv Kumar Kushawaha, Manish Majumder, Mahendra Singh Ashawat
A simple, sensitive, accurate, precise, and reproducible UV- spectrophotometric method and RP-HPLC methods were developed and validated for the estimation of Famotidine and Ofloxacin in bulk drug and pharmaceutical formulation. The Linearity regression was detected and shows a good linear relationship; in the concentration range of 10-50µg/mL (R2 >0.9908) for famotidine and 10-50µg/mL (r2>0.9913) for ofloxacin. The UV – spectrophotometric estimation was carried out by the first-order derivative spectrophotometric method and absorbance were recorded at 273 and 280nm. Beers range were found to be 5-50µg/mL, respectively for both drugs while, correlation coefficient r2 > 0.9988 and 0.9941 for famotidine and ofloxacin. The isoabsorptive point was found to be 274nm in HPLC optimized mobile phase composition, potassium dihydrogen orthophosphate: methanol (60:40). Chromatographic condition consisted of mobile phase potassium dihydrogen orthophosphate buffer pH 2.3, methanol (60:40v/v), run time 30 min, C-18 column (ODS Hypersil) and flow rate 0.8mL/minute. The retention time for famotidine and ofloxacin were found to be 2.44 min, 7.99 min. respectively, and detection at λmax 274nm for both drugs (overlain spectra). The UV methods and RP-HPLC showed good reproducibility and recovery with the percent relative standard deviation (RSD) less than 5%. As per ICH guidelines, the developed method was validated for linearity, accuracy, precision, Sandell's sensitivity, and repeatability proving its utility in the estimation of famotidine and ofloxacin in house tablet formulation.
建立了一种简便、灵敏、准确、精密度高、重现性好的紫外分光光度法和反相高效液相色谱法测定原料药和制剂中法莫替丁和氧氟沙星含量的方法。经线性回归检测,显示出良好的线性关系;法莫替丁的浓度范围为10 ~ 50µg/mL (R2 >0.9908),氧氟沙星的浓度范围为10 ~ 50µg/mL (R2 >0.9913)。采用一阶导数分光光度法进行紫外分光光度估计,在273和280nm处记录吸光度。两种药物的啤酒含量范围分别为5 ~ 50µg/mL,相关系数r2 >法莫替丁和氧氟沙星分别为0.9988和0.9941。在高效液相色谱优化的流动相正磷酸二氢钾:甲醇(60:40)中发现等吸收点为274nm。色谱条件为流动相正磷酸二氢钾缓冲液pH 2.3,甲醇(60:40v/v),运行时间30 min, C-18柱(ODS Hypersil),流速0.8mL/min。法莫替丁和氧氟沙星的保留时间分别为2.44 min和7.99 min,两种药物的最大检测波长为274nm(重叠光谱)。紫外法和反相高效液相色谱法重现性和回收率好,相对标准偏差(RSD)小于5%。根据ICH指南,建立的方法进行了线性、准确度、精密度、桑德尔灵敏度和重复性验证,证明了该方法可用于家用片中法莫替丁和氧氟沙星的含量估算。
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引用次数: 0
Development and Validation of UV Spectroscopy Method for the Determination of Posaconazole in Bulk and Formulation 紫外光谱法测定泊沙康唑原料药和制剂含量的建立与验证
Pub Date : 2023-09-07 DOI: 10.52711/2231-5675.2023.00027
Shivprasad Patil, Ajay Kshirsagar, Kartik Ade, Akash Bharkade, Madhav Bharkade, Ashish Birkalwar, Mahesh Chandolkar
The present study was undertaken to develop a spectrophotometric method for the determination of Posaconazole (PCZ) in pharmaceutical dosage forms. This paper describes a simple, rapid, accurate, and precise UV-spectrophotometric method for the assay of PCZin bulk and marketed dosage forms. The validation of the developed method was carried out according to ICH guidelines concerning linearity, precision, accuracy, specificity, the limit of detection, and the limit of quantification. The diluent is aqueous methanol. Calibration curves were obtained in the concentration range of 04-20µg/ml for PCZ and with good correlation coefficients (R2=0.9981). The precisions of the new method for the drug were less than the maximum allowable limit (%RSD < 2.0) specified by the ICH. Therefore, the method was found to be accurate, reproducible, and sensitive for the analysis of PCZ in pharmaceutical dosage forms.
建立了分光光度法测定制剂中泊沙康唑(PCZ)的方法。本文介绍了一种简单、快速、准确、精确的紫外分光光度法测定PCZin散装和市售剂型的方法。根据ICH指南对所建立的方法进行了关于线性、精密度、准确度、特异性、检出限和定量限的验证。稀释剂是甲醇水溶液。PCZ的浓度范围为04 ~ 20µg/ml,具有良好的相关系数(R2=0.9981)。新方法的精密度小于该药物的最大允许限度(%RSD <2.0)由ICH指定。结果表明,该方法准确、重现性好、灵敏度高,可用于药品剂型中PCZ的分析。
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引用次数: 0
Development and Validation of UV Spectroscopic Method for Simultaneous Estimation of Remogliflozin Etabonate and Vildagliptin in bulk and Pharmaceutical Dosage Form 紫外光谱法同时测定原料药和制剂中瑞格列净和维格列汀含量的建立与验证
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00012
Vashi Dhara, Chaudhari Hetvi
A new, simple, precise, accurate, reproducible, and efficient UV spectroscopic method was developed and validated for simultaneous estimation of Remogliflozin Etabonate and Vildagliptin in pure and pharmaceutical dosage form. The 𝜆max of Remogliflozin Etabonate and Vildagliptin in Methanol were found to be 236nm and 215nm, respectively. Calibration curves of Remogliflozin Etabonate and Vildagliptin were found to be linear in the concentration ranges of 5-25µg/mL and 1-5µg/mL with their correlation coefficient values (R2) 0.9993 and 0.9998, respectively. LOD and LOQ were found to be 0.0246µg/mL and 0.0745µg/mL for Remogliflozin Etabonate and 0.0278µg/mL and 0.0842µg/mL for Vildagliptin, respectively. In the precision study, the % RSD value was found within limits (RSD < 2%). The percentage recovery at various concentration levels varied from 99.25 to 101.06% for Remogliflozin Etabonate and 99.58 to 100.41% for Vildagliptin, respectively. The proposed method can be applied successfully for the simultaneous estimation of Remogliflozin Etabonate and Vildagliptin in pure and pharmaceutical dosage form. In this method simultaneous equation method was applied to find assay of both drugs in pharmaceutical dosage form.
建立了一种简便、精确、准确、重现性好、高效的紫外分光光度法,用于同时测定制剂制剂和制剂制剂remgliflozin Etabonate的含量。remgliflozin Etabonate和Vildagliptin在甲醇中的𝜆max分别为236nm和215nm。在5 ~ 25µg/mL和1 ~ 5µg/mL范围内,瑞格列净和维格列汀的校准曲线呈良好的线性关系,相关系数(R2)分别为0.9993和0.9998。regliflozin Etabonate的LOD和LOQ分别为0.0246µg/mL和0.0745µg/mL, Vildagliptin的LOD和LOQ分别为0.0278µg/mL和0.0842µg/mL。在精密度研究中,发现% RSD值在限定范围内(RSD < 2%)。在不同浓度下,瑞格列净的回收率为99.25 ~ 101.06%,维格列汀的回收率为99.58 ~ 100.41%。该方法可成功地同时测定制剂制剂和纯制剂remgliflozin Etabonate和维格列汀的含量。本方法采用联立方程法对两种药物的剂型进行测定。
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引用次数: 0
Recent Applications of UV-Visible Derivative Spectroscopic Method 紫外可见导数光谱法的最新应用
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00019
Amit J. Vyas, Harshal M. Vadile, Ajay I. Patel, Ashok B. Patel, Ashvin V. Dudhrejiya, Sunny R. Shah, Urvi J. Chotaliya, Devang B. Sheth
Derivative spectrophotometry is an analytical technique of great utility for extracting both qualitative and quantitative information from spectra composed of unresolved bands, and for eliminating the effect of baseline shifts and baseline tilts. Derivative spectrophotometry in the field of pharmaceutical analysis during the period 2018 – 2022 are reviewed. This paper draws attention to the fact that derivative treatment continues to be a promising tool for Multi-component Determination, Kinetic Studies, Pharmaceutical, clinical Analysis, Environmental fields of analysis or Food Analysis as it provides selective, validated, simple and cost-effective analytical method.
导数分光光度法是一种从未解析光谱中提取定性和定量信息的分析技术,用于消除基线偏移和基线倾斜的影响。综述了2018 - 2022年在药物分析领域的导数分光光度法。本文指出,衍生分析方法在多组分测定、动力学研究、药物、临床分析、环境分析或食品分析中仍然是一种有前途的工具,因为它提供了选择性、有效、简单和经济的分析方法。
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引用次数: 0
Method Development using a UV Visible Spectrophotometer for the Simultaneous Estimation of Rabeprazole, Aceclofenac and Paracetamol in Marketed Formulation 方法采用紫外可见分光光度法同时测定市售制剂中雷贝拉唑、乙酰氯芬酸和扑热息痛的含量
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00013
Wajid Ahmad, Rihan Jawed
Rheumatoid arthritis, or RA, is an autoimmune and inflammatory disease, which means that your immune system attacks healthy cells in your body by mistake, causing inflammation (painful swelling) in the affected parts of the body. RA mainly attacks the joints, usually many joints at once. A complexation, derivatization, extraction, evaporation and sensitive-free direct a new, simple, precise, accurate, reproducible, and efficient UV spectrophotometric method is developed and validated for the simultaneous estimation of ternary mixture of rabeprazole, (MET) aceclofenac (SXG) and paracetamol (DGF) in both their bulk form and combined in tablet dosage form recently approved by FDA in 2019 to be used for treatment of Type 2 diabetes mellitus by simultaneous equation method. The solutions of standard and sample were prepared in methanol: water (80:20 v/v). The 𝜆max for MET, SXG, and DGF were 232.0, 212.0 and 272.0nm, respectively. Calibration curves are linear in the concentration ranges 10-50𝜇g/ml for MET, 1-5𝜇g/ml for SXG and 5-25𝜇g/ml for DGF, respectively. Results of analysis of simultaneous equation method were analyzed and validated for various parameters according to ICH guidelines.
类风湿性关节炎,简称RA,是一种自身免疫和炎症性疾病,这意味着你的免疫系统会错误地攻击你体内的健康细胞,导致身体受影响部位的炎症(疼痛的肿胀)。类风湿性关节炎主要攻击关节,通常是同时攻击多个关节。建立了一种新的、简单、精确、准确、可重复、高效的紫外分光光度法,用于同时测定FDA于2019年批准用于治疗2型糖尿病的雷贝拉唑(MET)、醋氯芬酸(SXG)和扑热息痛(DGF)的原装和片剂混合物。用甲醇:水(80:20 v/v)配制标准品和样品溶液。MET、SXG和DGF的𝜆max分别为232.0、212.0和272.0nm。MET浓度范围为10-50𝜇g/ml, SXG浓度范围为1-5𝜇g/ml, DGF浓度范围为5-25𝜇g/ml,校准曲线呈线性关系。根据ICH指南对联立方程法的分析结果进行了分析和验证。
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引用次数: 0
A Review of HPLC Method Development and Validation as per ICH Guidelines 根据ICH指南的HPLC方法开发和验证综述
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00024
Akash D. Rajmane, Komal P. Shinde
Method development and validation are continuous processes that progress in parallel with the evolution of drug products. Changes encountered during drug development may require modifications to existing analytical methods. These modifications to the methods, in turn, may require additional validation. The advent of new techniques and improved instrumentation in the field of analysis may give way to more sensitive, precise, and accurate methods if the existing methods are erratic or unreliable; time-consuming, or too expensive. Thus, continuous new analytical method development and validation activities are essential for the growing drug development programs.
方法开发和验证是连续的过程,与药品的发展同步进行。在药物开发过程中遇到的变化可能需要修改现有的分析方法。反过来,对方法的这些修改可能需要额外的验证。如果现有方法不稳定或不可靠,分析领域新技术和改进仪器的出现可能会让位于更灵敏、更精确和更准确的方法;耗时,或者太贵。因此,持续的新分析方法开发和验证活动对于不断增长的药物开发计划至关重要。
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引用次数: 0
A Review UV Method Development and Validation 紫外检测方法发展与验证综述
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00021
Komal P. Shinde, Akash D. Rajmane
Ultraviolet spectroscopy is one important and advanced analytical instrument in the Pharmaceutical industry and used for the last 35 years. The method of analysis is based on measuring the absorption of monochromatic light by colorless compounds in the near-ultraviolet path of the spectrum (200-400nm). The pharmaceutical analysis comprises the procedures necessary to determine such compounds' “identity, strength, quality, and purity”. It also includes the analysis of raw materials and intermediates during the manufacturing process of drugs. The fundamental principle of operation of a spectrophotometer covering the UV region consists that light of a definite interval of wavelength passes through a cell with solvent and falls onto the photoelectric cell that transforms the radiant energy into electrical energy measured by a galvanometer. Ultraviolet-visible spectroscopy is used to obtain the absorbance spectra of a compound in solution or as a solid.
紫外光谱法是制药工业中一种重要的先进分析仪器,已有35年的历史。分析方法是基于测量光谱近紫外路径(200-400nm)中无色化合物对单色光的吸收。药物分析包括确定这些化合物的“特性、强度、质量和纯度”所需的程序。它还包括药品生产过程中对原料和中间体的分析。覆盖紫外线区域的分光光度计的基本工作原理是,一定波长间隔的光通过带有溶剂的电池,并落在光电电池上,光电电池将辐射能转化为由电流计测量的电能。紫外-可见光谱学用于测定化合物在溶液或固体状态下的吸光度。
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引用次数: 0
Review on Stability Indicating Assay Method or Forced Degradation Study: Strategy and Regulatory Consideration 稳定性指示测定方法或强制降解研究综述:策略和监管考虑
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00022
Amit J. Vyas, Chirag D. Jadav, Ajay I. Patel, Ashok B. Patel, Sunny R. Shah, D. Sheth, S. Dholakia
Stability-indicating methods are crucial analytical techniques that aim to evaluate the stability of a drug substance or product over time. They are designed to detect any alterations in the drug's chemical, physical, or biological characteristics that may occur during storage, transportation, and usage. These modifications can significantly impact the drug's safety and effectiveness, making stability testing an integral part of pharmaceutical quality control. The stability-indicating methods are used to identify the degradation products of a drug, quantify the rate of degradation, and determine the factors that may contribute to degradation. These conditions can include exposure to light, heat, humidity, and various chemical and physical stressors. The methods can be chromatographic or spectrophotometric and undergo validation to ensure their reliability, accuracy, and specificity for the specific drug. The acceptable level of degradation in forced degradation studies should not exceed 5-30% of the total active ingredient present in the drug substance or product. This helps to ensure that the results obtained are trustworthy and can be used to make informed decisions about the stability of the drug.
稳定性指示方法是评价原料药或制剂随时间变化的稳定性的关键分析技术。它们的目的是检测在储存、运输和使用过程中可能发生的药物的化学、物理或生物特性的任何变化。这些修饰可以显著影响药物的安全性和有效性,使稳定性测试成为药品质量控制的一个组成部分。稳定性指示方法用于识别药物的降解产物,量化降解速率,并确定可能导致降解的因素。这些条件包括暴露于光、热、湿和各种化学和物理压力。这些方法可以是色谱法或分光光度法,并经过验证以确保其对特定药物的可靠性,准确性和特异性。强制降解研究中可接受的降解水平不应超过原料药或制剂中总活性成分的5-30%。这有助于确保获得的结果是可信的,并可用于对药物的稳定性做出明智的决定。
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引用次数: 0
Bio-Chemical Analysis of Pachai Karpoora Mathirai Pachai Karpoora Mathirai的生化分析
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00023
R. Saraswathi, A. Elavarasi
Siddha system of medicine is ancient and traditional medicine based on pancha bootha theory and taste based medicine. Human body also based on pancha bootha theory, any imbalance in pancha bootham in human body alter the three vital humors (Vatham, Pitham and Kabam) causes disesease in human.20 So human disease can be treated with panchabootha theory based siddha drugs. Pacchai Karpoora mathirai is siddha medicine used for treating all type of fever (Suram) Especially kabasuram. Kabasuram is a siddha term more are less co related to Bronchitis in modern aspect of medicine in pediatric age group. Author decided to use a Pacchai karpoora mathirai for treating the kabasuram (Bronchitis) based on ingridients in the drug.13,14,15,16,17. The bio-chemical analysis of Pacchai Karpoora Mathirai was done in Biochemistry lab, National Institute of siddha, Chennai-47. Preliminary qualitative phytochemical screening was done by Kolkate (1) method. The bio-chemical analysis shows the presence of Carbonate, Aluminium, Zinc, Magnesium.
悉达医学体系是一种古老的传统医学,以pancha bootha理论和味觉医学为基础。人体也基于pancha bootha理论,人体pancha bootha的任何不平衡都会改变人体的三种重要体液(Vatham, Pitham和Kabam),从而导致人体疾病所以人类的疾病可以用基于释迦理论的药物来治疗。Pacchai Karpoora mathirai是用于治疗各种发烧(Suram)的悉陀药,尤其是kabasuram。Kabasuram是一个独立的术语,在现代儿科医学中与支气管炎的关系较少。根据该药的成分,作者决定使用Pacchai karpoora mathirai治疗支气管炎(kabasuram)。Pacchai Karpoora Mathirai的生化分析是在金奈-47国家siddha研究所生物化学实验室完成的。采用Kolkate(1)法进行初步的植物化学定性筛选。生化分析显示碳酸盐,铝,锌,镁的存在。
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引用次数: 0
A New Zero Cross Technique for Simultaneous Estimation of Rosuvastatin Calcium and Fenofibrate in Tablets by UV Derivative Spectroscopic Method 零交叉紫外导数光谱法同时测定瑞舒伐他汀钙和非诺贝特片剂的含量
Pub Date : 2023-06-03 DOI: 10.52711/2231-5675.2023.00017
M. Pranati, N. Rani, B. Pravallika
A Simple and reliable Zero cross technique for simultaneous estimation of Rosuvastatin Calcium and Fenofibrate in tablets by using UV derivative method was developed. The quantitative determination of the drugs was carried out using the Zero cross values measured at 235nm and 273nm for Rosuvastatin Calcium and Fenofibrate respectively. The Calibration curves constructed at these wavelengths for the determination of the linearity in the concentration range of 5-25µg/mlfor both the selected drugs. The low relative standard deviation values indicate good precision and higher recovery values indicate accuracy of the proposed method. The developed zero cross technique was found to be simple, accurate, precise, specific, sensitive and reproducible which can be directly and easily applied tomarketed formulations.
建立了紫外导数法同时测定瑞舒伐他汀钙和非诺贝特片剂中瑞舒伐他汀钙和非诺贝特含量的零交叉技术。瑞舒伐他汀钙和非诺贝特分别采用235nm和273nm处的零交叉值进行定量测定。在所选药物在5 ~ 25µg/ml浓度范围内建立了校准曲线,用于确定两种药物的线性关系。相对标准偏差值较低,表明该方法的精密度较好;相对标准偏差值较高,表明该方法的准确度较高。该方法简便、准确、精密度高、专属性好、灵敏度高、重现性好,可直接应用于市场制剂中。
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引用次数: 0
期刊
Asian Journal of Pharmaceutical Analysis
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