Pharmaceutical Methods最新文献_第10页

Simultaneous Determination of Cefepime and Tazobactam in Injectables by Ultra-High Performance Liquid Chromatography Method 超高效液相色谱法同时测定注射液中头孢吡肟和他唑巴坦的含量

Pharmaceutical Methods Pub Date : 2014-07-18 DOI: 10.5530/PHM.2014.1.4

B. Shrestha, N. Bhuyan, B. N. Sinha

{"title":"Simultaneous Determination of Cefepime and Tazobactam in Injectables by Ultra-High Performance Liquid Chromatography Method","authors":"B. Shrestha, N. Bhuyan, B. N. Sinha","doi":"10.5530/PHM.2014.1.4","DOIUrl":"https://doi.org/10.5530/PHM.2014.1.4","url":null,"abstract":"Aim: Stability indicating ultra-high performance liquid chromatography (UHPLC) method was developed and validated for the determination of cefepime (CFPM) and tazobactam (TZB) in injectable dosage form. Materials and Methods: Separation was performed in a Dionex Ultimate 3000 UPHLC system equipped with chromeleon software using Acclaim 120 C 18 (250 × 4.6 mm, 5 μm particle size) column with mobile phase (pH 6.0) containing methanol and sodium acetate buffer in the ratio of 11:89 v/v with a fl ow rate of 1.8 mL/min and detection wavelength of 220 nm. Stress studies were performed using HCL, NaOH, H 2 O 2 , and ultraviolet radiation. Results: The method was found to be linear in the concentration range of 50-350 μg/ml (R 2 = 0.998) and 6.25-43.75 μg/ml (R 2 = 0.998) with the regression equation y = 11068 x + 115231 and y = 8317.1x – 9869.7 for CFPM and TZB, respectively. The percentage of relative standard deviation (%RSD) of 0.63 and 1.39 for intra-day and 0.64 and 0.54 for inter-day precision, respectively for CFPM and TZB suggest the precision of the method as all these values are Conclusion: The method was found to be accurate, precise, specifi c, robust, linear, and stability indicating for the determination of CFPM and TZB in injectable dosage form. Key words: Cefepime, injectables, simultaneous determination, tazobactam, ultra high performance liquid chromatography.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"8 1","pages":"20-26"},"PeriodicalIF":0.0,"publicationDate":"2014-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74433394","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 5

Analytical Method Development and Validation of Metformin, Voglibose, Glimepiride in Bulk and Tablet Dosage Form by Gradient RP-HPLc 梯度反相高效液相色谱法建立二甲双胍、伏格列糖、格列美脲散装和片剂的分析方法及验证

Pharmaceutical Methods Pub Date : 2014-07-18 DOI: 10.5530/PHM.2014.1.5

K. Neelima, Y. R. Prasad

{"title":"Analytical Method Development and Validation of Metformin, Voglibose, Glimepiride in Bulk and Tablet Dosage Form by Gradient RP-HPLc","authors":"K. Neelima, Y. R. Prasad","doi":"10.5530/PHM.2014.1.5","DOIUrl":"https://doi.org/10.5530/PHM.2014.1.5","url":null,"abstract":"Background: A simple, sensitive, linear, precise, and accurate method by gradient reversed-phase-high performance liquid chromatography for the simultaneous estimation of metformin (MET), voglibose (VOG) and glimepiride (GLI) in bulk and in their combined tablet dosage form was developed and validated. Materials and Methods: The separation of the three drugs was based on the use of Inertsil ODS 3V (150 × 4.6 mm, i.e. 5 μm) column in a gradient mode. Mobile phase consisted of 0.02 M Phosphate buffer adjusted to pH 2.5 using dilute orthophosphoric acid (solvent A) and acetonitrile (solvent B) was set with gradient programming for 18 min and was delivered at 1 ml/min fl ow rate and effl uents are achieved with variable wavelength: Photodiode array detector at 230 nm. Results: The retention times of MET, VOG, and GLI were found to be 2.423, 8.191, and 11.708, respectively. The percentage assay of MET, VOG, and GLI was found to be 99.92%, 99.32, and 99.72%, respectively. Calibration curves were linear for MET, VOG and GLI at concentration ranges of 200-600 μg/ml, 0.08-0.24 μg/ml, and 0.8-2.4 μg/ml with the regression coeffi cient of 0.999 for all the three drugs and precise with (% relative standard deviation Conclusion: The method was validated by determining its linearity, accuracy, precision, system suitability and can be employed for routine quality control analysis as per International Conference on Harmonization guidelines. Key words: Glimepiride, gradient reversed-phase-high performance liquid chromatography, International Conference on Harmonization guidelines, metformin, validation, voglibose.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"42 1","pages":"27-33"},"PeriodicalIF":0.0,"publicationDate":"2014-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75187171","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 9

A Validated Quantitative Estimation and Stability Indicating Reversed-phase-high Performance Liquid Chromatography Method for Balofl oxacin in Bulk and its Tablet Formulation 巴洛弗沙星原料药及其片剂的反相高效液相色谱定量评价及稳定性研究

Pharmaceutical Methods Pub Date : 2014-07-18 DOI: 10.5530/PHM.2014.1.1

A. Dacha, K. Prakash

{"title":"A Validated Quantitative Estimation and Stability Indicating Reversed-phase-high Performance Liquid Chromatography Method for Balofl oxacin in Bulk and its Tablet Formulation","authors":"A. Dacha, K. Prakash","doi":"10.5530/PHM.2014.1.1","DOIUrl":"https://doi.org/10.5530/PHM.2014.1.1","url":null,"abstract":"This paper describes the development of a stability-indicating reversed-phase-high performance liquid chromatography (RP-HPLC) method for balofl oxacin (BFX) in the presence of its degradation products generated from forced decomposition studies. The drug substance was found to be susceptible to stress conditions of acid, base, oxidation, wet heat, and photo degradation. The drug was found to be stable to the dry heat condition attempted. Successful separation of the drug from the degradation products formed under stress conditions was achieved on a Zorbax C 18 column (150 mm × 4.6 mm id, 5 microns particle size) using methanol-water pH adjusted to 2.5 by orthophosphoric acid (40:60, v/v) as the mobile phase at a fl ow rate of 0.5 mL/min at 30°C temperature. Quantifi cation was achieved with photodiode array detection at 293 nm over the concentration range 50-150 μg/ml with mean recovery of 100.0 ± 0.53% for BFX by the RP-HPLC method. Statistical analysis proved the method is repeatable, specifi c, and accurate for estimation of BFX. Because the method could effectively separate the drug from its degradation products, it can be used as a stability-indicating method. Key words: Balofl oxacin, reversed-phase-high performance liquid chromatography, orthophosphoric acid, validation.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"6 1","pages":"1-6"},"PeriodicalIF":0.0,"publicationDate":"2014-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83151844","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 4

Development and Application of Liquid Chromatographic Method for Simultaneous Determination of Elvitegravir, Tenofovir Disoproxil Fumarate, Emtricitabine, and Cobicistat in Fixed Dosage Form 液相色谱法同时测定固定剂型依维替韦、富马酸替诺福韦、恩曲他滨和可比司他的含量及应用

Pharmaceutical Methods Pub Date : 2014-07-18 DOI: 10.5530/PHM.2014.1.2

Raghu Ram Jampala, V. Kiran Kumar, Appala Raju Nemala

{"title":"Development and Application of Liquid Chromatographic Method for Simultaneous Determination of Elvitegravir, Tenofovir Disoproxil Fumarate, Emtricitabine, and Cobicistat in Fixed Dosage Form","authors":"Raghu Ram Jampala, V. Kiran Kumar, Appala Raju Nemala","doi":"10.5530/PHM.2014.1.2","DOIUrl":"https://doi.org/10.5530/PHM.2014.1.2","url":null,"abstract":"Quad pill is fi xed-dose combinations containing four drugs in a single tablet with the intention of reducing the number of tablets that need to be taken. Elvitegravir (ELVT)/cobicistat (COB)/emtricitabine (EMCB)/tenofovir disoproxil fumarate (TDF) is a complete regimen intended for treatment of HIV infection. Developing a single analytical method for the estimation of individual drugs in a QUAD is very challenging, due to the formation of drug-drug and drug-excipient interactions. The present study demonstrates the applicability of chromatographic method to develop a new, sensitive, single high-performance liquid chromatography method for the simultaneous quantitative determination of four antiviral agents in fi xed pharmaceutical dosage form. Chromatographic separation of the four antiviral drugs was achieved by using a gradient elution at a fl ow rate of 1.0 ml/min on Inertsil ODS 3V C 18 column (250 m × 4.6 mm, 5 μm particle size, 100 A pore size) at ambient temperature. Mobile phase A of the gradient solvent system was KH 2 PO 4 (0.02 M) in 1000 ml of water and by adjusting the pH to 2.5 with dilute orthophosphoric acid and mobile phase B was acetonitrile. Ultraviolet detection at 240 nm was employed to monitor the analytes. A linear response was observed for EMCB over the concentration range 20-240 μg/ml, for TDF over the concentration range of 30-360 μg/ml, for ELVT and COB over the concentration range of 15-180 μg/ml. Limit of detection for EMCB, TDF, ELVT, and COB were 0.02 μg/ml, 0.03 μg/ml, 0.75 μg/ml, and 3 μg/ml, respectively. Limit of quantifi cation for EMCB, TDF, ELVT, and COB were 0.06 μg/ml, 0.09 μg/ml, 2.25 μg/ml, and 9 μg/ml respectively. Key words: Cobicistat, elvitegravir, emtricitabine, gradient-high performance liquid chromatography, quadpill, tenofovir disoproxil fumarate.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"75 1","pages":"7-13"},"PeriodicalIF":0.0,"publicationDate":"2014-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86791823","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 18

Exploring the Use of Sodium Benzoate as Hydrotrope for the Estimation of Lornoxicam in their Marketed Formulation 探索使用苯甲酸钠作为水变性物对氯诺昔康市售制剂进行评估

Pharmaceutical Methods Pub Date : 2014-07-18 DOI: 10.5530/PHM.2014.1.3

T. Shukla, P. Khare, N. Thakur, V. Dhote, H. S. Chandel, S. Pandey

{"title":"Exploring the Use of Sodium Benzoate as Hydrotrope for the Estimation of Lornoxicam in their Marketed Formulation","authors":"T. Shukla, P. Khare, N. Thakur, V. Dhote, H. S. Chandel, S. Pandey","doi":"10.5530/PHM.2014.1.3","DOIUrl":"https://doi.org/10.5530/PHM.2014.1.3","url":null,"abstract":"Increasing the aqueous solubility of insoluble drugs is of major importance for the estimation by spectrophotometric technique. Various techniques have been employed to enhance the aqueous solubility of poorly water soluble drugs. Hydrotropic solubilization is one of them. In the present study, sodium benzoate was chosen as hydrotrope to enhance the solubility of Lornoxicam for its spectrophotometric estimation in their marketed formulation. Preliminary solubility of Lornoxicam, spectral study, method development and its validation was done as per ICH guidelines. Solubility study of Lornoxicam displayed a signifi cant increment in the solubility due to 10% solution of sodium benzoate which will be suffi cient to extract the drug from its dosage form. The sample solution has shown the λ max at 376 nm and obeys the lambert beer law in the concentration range of 5-25 μg/ml with a correlation coeffi cient of 0.999. The accuracy of the method was proved by recovery study with mean recovery of 99.87. Precision study also shows no signifi cant deviation from the mean value. A limit of detection and limit of quantitation result indicates the sensitivity of the method with the values 1.02 μg/ml and 3.39 μg/ml simultaneously. Hence, the methodology can be used safely and effectively for the routine estimation of Lornoxicam in the bulk drug and marketed formulation. Key words: Hydrotropic solubilization, sodium benzoate, spectrophotometric estimation, validation.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"57 1","pages":"14-19"},"PeriodicalIF":0.0,"publicationDate":"2014-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73812354","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Development and Validation of UV Spectrophotometric Method for the Estimation of Kaempferol in Kaempferol: Hydrogenated Soy PhosphatidylCholine (HSPC) Complex 紫外分光光度法测定山奈酚氢化大豆磷脂酰胆碱(HSPC)配合物中山奈酚含量的建立与验证

Pharmaceutical Methods Pub Date : 2014-07-18 DOI: 10.5530/PHM.2014.1.6

D. Telange, A. Patil, A. Tatode, Bhushan S. Bhoyar

{"title":"Development and Validation of UV Spectrophotometric Method for the Estimation of Kaempferol in Kaempferol: Hydrogenated Soy PhosphatidylCholine (HSPC) Complex","authors":"D. Telange, A. Patil, A. Tatode, Bhushan S. Bhoyar","doi":"10.5530/PHM.2014.1.6","DOIUrl":"https://doi.org/10.5530/PHM.2014.1.6","url":null,"abstract":"Introduction: Kaempferol (3,5,7-trihydroxy-2-(4-hydroxyphenyl)-4H-1-benzopyran-4-one) is a natural flavonoid belongs to subcategory of flavonol family. The Kaempferol – Hydrogenated Soy Phosphatidylcholine (HSPC) Complex was obtained by refluxing and freeze drying method. UV – Visible Spectrophotometric method has been developed for determination of Kaempferol in Kaempferol – HSPC Complex. Objective: A validated UV – Visible spectrophotometric method for determination of Kaempferol in Kaempferol – HSPC complex. Methods: The Kaempferol – HSPC Complex (Phytosomes) were prepared by dissolving both Kaempferol and Hydrogenated Soy Phosphatidylcholine (HSPC) in 1, 4 – dioxane for refluxing up to 2h and freeze dried. The spectrophotometric detection of kaempferol was done at absorption maximum (λmax) of 365 nm and 265 nm using methanol as solvent. The developed method was validated as per ICH guidelines. Result: The Kaempferol content in Kaempferol – HSPC Complex was found to be 79.32% and 79.19% at 365 nm and 265 nm. Kaempferol demonstrated good linearity in concentration range of 2 – 12 µg/ml (r2>0.99) at 365 nm and 2 – 14 µg/ml (r 2 >0.99) at 265nm. Precision and mean recoveries were found to be in the range of (% RSD 0.0957 & 0.0580) and (% RSD 0.1461 & 0.0959) and 99.70 % & 91.85 % at 365 nm and at 265 nm. LOD and LOQ were found to be (0.015µg/ml & 0.0191µg/ml) and (0.0457µg/ml & 0.0579µg/ml) respectively. Conclusion: The developed method was found to be simple, specific, economic, reliable, accurate, precise, reproducible and used as a quality control tool for analysis of Kaempferol. Key Words: Freeze drying, HSPC, Kaempferol, Method validation, UV – Visible spectrophotometer.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"41 1","pages":"34-38"},"PeriodicalIF":0.0,"publicationDate":"2014-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88376666","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 17

A Validated RP-HPLC-UV Method for Identification of Reference Standards of Degradation Products of Fenofibrate 非诺贝特降解产物标准品的RP-HPLC-UV鉴别方法

Pharmaceutical Methods Pub Date : 2014-01-01 DOI: 10.5530/PHM.2014.2.6

S. Mulgund, S. Anbazhegan, B. P. Pawaskar, S. Gabhe

{"title":"A Validated RP-HPLC-UV Method for Identification of Reference Standards of Degradation Products of Fenofibrate","authors":"S. Mulgund, S. Anbazhegan, B. P. Pawaskar, S. Gabhe","doi":"10.5530/PHM.2014.2.6","DOIUrl":"https://doi.org/10.5530/PHM.2014.2.6","url":null,"abstract":"Background: During the stress degradation studies of Fenofibrate the structures of two major degradation products, namely 2-[4-(4-chlorobenzoyl)phenoxy]-2-methyl propanoic acid and methyl 2-[4-(4-chlorobenzoyl)phenoxy]-2-methylpropanoate, were characterized using LC-MS/MS studies under alkaline and acidic hydrolytic conditions, respectively. The present communication deals with synthesis, spectral characterization and further application of those reference standards of degradation products in identification of degradation products in bulk sample of drug through retention time matching studies. Methods: The reference standards of the degradation products were synthesized in the laboratory and their identity were confirmed using spectral studies. These were employed for retention matching studies using HPLC studies. The chromatographic conditions were as follows: stationary phase: Waters X Bridge C 18 column (250x4.6 mm, internal diameter, particle size 5 μm), mobile phase: acetonitrile: water in 75:25 v/v, column oven temperature: ambient, proportion. The chromatograms were monitored at 286 nm with a flowrate of 1 mL/min. The method was validated according to the ICH. guidelines. Results: Retention time values of synthesized reference standards were found to be identical with retention time values of those degradation products in stressed samples. The calibration curves showed good linear regression (r 2 >0.999) within test ranges. The method showed good reproducibility and sensitivity for quantification of both degradation products in samples. Method was precise and %recovery of both reference products was within 98-102%. Conclusion: This communication emphasizes use of non-compendial reference standards for quantification of degradation products by chromatographic methods. Quantitative validation parameters like Limit of detection and Limit of quantitation were established. Key words: Degradation impurities, Fenofibrate, Non-compendial reference standards, RP-HPLC, Retention time matching.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"26 1","pages":"79"},"PeriodicalIF":0.0,"publicationDate":"2014-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81358817","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

An Overview of Liquid Chromatography-Mass Spectroscopy Instrumentation 液相色谱-质谱仪器概述

Pharmaceutical Methods Pub Date : 2014-01-01 DOI: 10.5530/PHM.2014.2.2

S. Parasuraman, R. Anish, S. Balamurugan, S. Muralidharan, Kalaimani Jayaraja Kumar, V. Vijayan

{"title":"An Overview of Liquid Chromatography-Mass Spectroscopy Instrumentation","authors":"S. Parasuraman, R. Anish, S. Balamurugan, S. Muralidharan, Kalaimani Jayaraja Kumar, V. Vijayan","doi":"10.5530/PHM.2014.2.2","DOIUrl":"https://doi.org/10.5530/PHM.2014.2.2","url":null,"abstract":"Chromatography is a separation technique used to separate the individual compound from a mixture using a stationary and mobile phase. Discovery of chromatography is a millstone event in biomedical research. Chromatographic separation is based on the principles of adsorption, partition, ion exchange, molecular exclusion, affinity and Chirality. There are many types of chromatography available for quantitative and qualitative analysis of pharmaceutical agents, which includes Liquid Chromatography-Mass Spectrometry (LC-MS). Combination of chromatography with spectrometry is first reported in 1967 and first LC-MS system was introduced in 1980s. LC-MS is an analytical chemistry technique that combines the physical separation capabilities of liquid chromatography with the mass analysis and mass spectrometry. Mainly the LC-MS contains liquid chromatography assembly, ion generation unit/ ionization source, mass analyzer and mass spectrometric data acquisition. LC-MS is most commonly used in biomedical sciences for pharmacokinetic analysis, genetic analysis, structural elucidation, etc. The main objective of this review is to overview the principle, instrumentation and application of LC-MS. Key words: Analysis, Chromatography, HPLC-MS, LC-MS.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"119 1","pages":"47"},"PeriodicalIF":0.0,"publicationDate":"2014-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91535038","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 18

RP-HPLC Method Development and Validation for the Simultaneous Determination of Clindamycin and Miconazole in Pharmaceutical Dosage Forms 药品剂型中克林霉素和咪康唑同时测定的反相高效液相色谱法建立及验证

Pharmaceutical Methods Pub Date : 2014-01-01 DOI: 10.5530/PHM.2014.2.3

Venkata R. Prava, G. Seru

{"title":"RP-HPLC Method Development and Validation for the Simultaneous Determination of Clindamycin and Miconazole in Pharmaceutical Dosage Forms","authors":"Venkata R. Prava, G. Seru","doi":"10.5530/PHM.2014.2.3","DOIUrl":"https://doi.org/10.5530/PHM.2014.2.3","url":null,"abstract":"Objective: A simple, precise, reliable, rapid and reproducible reversed phase–high-performance liquid chromatography method was developed and validated for the simultaneous estimation of Clindamycin (CDM) and Miconazole (MCZ) present in tablet dosage forms. Method: Chromatographic separation achieved isocratically on Inertsil ODS C 18 (250x4.6 mm, 5 mm) column and buffer (pH 3.5) and acetonitrile (65:35 v/v) as mobile phase, at a flow rate of 1 ml/min. Detection was carried out at 220 nm. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the ICH guidelines. Results: The retention times for CDM and MCZ was found to be 2.2 and 3.2 min, respectively. Linearity for CDM and MCZ was in the range of 5-30 μg/ml and 10-60 μg/ml, respectively. The mean recoveries obtained for CDM and MCZ were 99.73 ± 0.8 and 100.2 ± 0.58%, respectively, and Relative standard deviation (RSD) was less than 2. The correlation coefficients for all components are close to 1. The RSDs for three replicate measurements in three concentrations of samples in tablets are always less than 2%. Conclusion: Developed method was found to be accurate, precise, selective and rapid for simultaneous estimation of CDM and MCZ in tablets. Key words: Clindamycin, Miconazole, RP-HPLC, Simultaneous estimation, Tablets.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"59 1","pages":"56"},"PeriodicalIF":0.0,"publicationDate":"2014-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76498916","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 3

Development and Validation of RP-HPLC Method with Diode Array Detection for Estimation of Metaxalone in Rat Plasma 二极管阵列反相高效液相色谱法测定大鼠血浆中甲他龙含量的建立与验证

Pharmaceutical Methods Pub Date : 2014-01-01 DOI: 10.5530/PHM.2014.2.4

I. Rizwana, K. Prakash, G. Mohan

{"title":"Development and Validation of RP-HPLC Method with Diode Array Detection for Estimation of Metaxalone in Rat Plasma","authors":"I. Rizwana, K. Prakash, G. Mohan","doi":"10.5530/PHM.2014.2.4","DOIUrl":"https://doi.org/10.5530/PHM.2014.2.4","url":null,"abstract":"Purpose: To develop a simple, highly sensitive, precise and accurate high-performance liquid chromatographic method with photodiode array detection and validated for the rapid quantification of metaxalone in rat plasma samples. Method: Following Liquid-Liquid Extraction (LLE), metaxalone and the internal standard Phenytoin (PHY) were extracted from an aliquot of 200 mL of plasma. Chromatographic separation was carried out using Phenomenex Luna C 8 column (250 mmμ 4.6 mmμ 5 mm) with mobile phase composed of phosphate buffer, pH 7 and acetonitrile in 35:65, v/v ratio. The analyte was monitored with UV detector at 219 nm. The developed method was validated with respect to linearity, accuracy, precision, specificity and stability. The peak area ratio of MET to that of internal standard, PHY was used for the quantification of samples. Results: The retention time of MET and PHY were found to be 2.30 and 3.02 min respectively. The calibration curve was linear (r 2 > or=0.99) ranging from 1.505-538.254 ng/ml and the lower limit of quantification was 1.505 ng/mL. Interday and Intraday precision were lower than 5% (CV) and accuracy ranged from 95 to 105% in terms of percent accuracy. Mean extraction recovery was found to be above 94%. Conclusion: A simple, alternative, reproducible and sensitive HPLC-DAD method was developed for MET that can be used in preclinical pharmacokinetics. Key words: Ammonium formate buffer, Acetonitrile, Metaxalone, Phenytoin, Preclinical pharmacokinetics.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"18 1","pages":"61"},"PeriodicalIF":0.0,"publicationDate":"2014-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85626721","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1