Pharmaceutical Methods最新文献

Validated RP-HPLC Method Development of Pazopanib in Bulk and its Pharmaceutical Dosage Form 帕唑帕尼原料药及其剂型的反相高效液相色谱法研究

Pharmaceutical Methods Pub Date : 2020-09-25 DOI: 10.5530/PHM.2020.1.4

Kiran Kumar Buralla, V. Parthasarathy

{"title":"Validated RP-HPLC Method Development of Pazopanib in Bulk and its Pharmaceutical Dosage Form","authors":"Kiran Kumar Buralla, V. Parthasarathy","doi":"10.5530/PHM.2020.1.4","DOIUrl":"https://doi.org/10.5530/PHM.2020.1.4","url":null,"abstract":"Objectives: An accurate, sensitive, precise and rapid method for analysis and quantification of Pazopanib by Reverse Phase High Performance Chromatography (RP-HPLC) was developed and validated. Pazopanib in bulk and formulations were analyzed and quantification. Methods: Pazopanib in bulk and formulations were analyzed on Phenomenex enable C18 column (15x4.6mm, 5μm particle size) as stationary phase. Mobile phase was composed of acetonitrile and phosphate buffer (pH 5) in the ratio of 60:40%v/v at a flow rate of 1.2ml/min. elutes were analyzed using PDA detector at a detection wavelength of 290nm. The proposed method was validated by ICH guidelines, Validation of Analytical Procedures: Text and Methodology Q2 (R1). Results: In this study, the chromatographic peaks of Pazopanib showed good resolution with retention time of 2.190min. Pazopanib showed an excellent linearity with 0.998 of correlation coefficient. Other validation parameters including precision, specificity, accuracy and robustness demonstrated good reliability in the quantification of Pazopanib. Conclusion: Thus the newly developed and validated method can be conveniently used for the quantification of Pazopanib in bulk and formulation. The method can also be applied to multi-component drug analysis.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"44 1","pages":"21-24"},"PeriodicalIF":0.0,"publicationDate":"2020-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83248441","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: 0

A New HPTLC Method for Analysis of Artemisinin Derivatives (Artemether and Lumefantrine) in Bulk Drug and Liposomal Formulation: Stress Degradation Study 高效液相色谱法分析原料药和脂质体制剂中青蒿素衍生物(蒿甲醚和氨芳汀)的应力降解研究

Pharmaceutical Methods Pub Date : 2020-09-25 DOI: 10.5530/PHM.2020.1.3

A. Rahman, R. Harwansh, Kashif Shakeel

引用次数: 0

Analytical Validation and Stability Indicating Studies for Simultaneous Estimation of Benidepine and Metoprolol by Strong Cation Exchange (SCX) Chromatography 强阳离子交换(SCX)色谱法同时测定贝尼地平和美托洛尔的分析验证及稳定性指示研究

Pharmaceutical Methods Pub Date : 2020-09-25 DOI: 10.5530/PHM.2020.1.2

K. B. Gabhane, D. B. Kamdi, C. A. Gulhane, Pankaj Kharabe

{"title":"Analytical Validation and Stability Indicating Studies for Simultaneous Estimation of Benidepine and Metoprolol by Strong Cation Exchange (SCX) Chromatography","authors":"K. B. Gabhane, D. B. Kamdi, C. A. Gulhane, Pankaj Kharabe","doi":"10.5530/PHM.2020.1.2","DOIUrl":"https://doi.org/10.5530/PHM.2020.1.2","url":null,"abstract":"Introduction: Polar anti-hypertensive drugs like benidepine and metoprolol often suffer from peak fronting and peak tailing effects in RP-HPLC. SCX chromatography which is alternative and complimentary to this RP-HPLC also has the capability to separate benidepine and metoprolol. Considering these aspects, SCX method was developed with performing stability indicating studies for the simultaneous quantification of benidepine (BEN) and metoprolol (MET) in bulk and tablet formulation. Methods: This investigation was performed on the Phenomenex Luna SCX column (100 × 2.1 mm, ID, particle size 5 μm) where both BEN and MET were eluted with ammonium formate (15mM) buffer: MeOH in ratio of 75:25 v/v for 12 min with isocratic elution at the flow rate of 1.2 ml/min; performed at 28°C and monitored at 226 nm wavelength. Results: The average retention time of BEN and MET were 1.290 and 3.520 min, respectively. The validation studies revealed good linearity over different concentration ranging between 7.5-250 μg/ml for BEN and 15.5-250 μg/ml for MET with R2 values were 0.999 recorded for both drugs. Average drug recoveries of BEN and MET were ranging between 99.36±0.83% and 100.51±1.03%, respectively. The acid (0.1N HCl; 50°C), dry heat (50°C) and alkali (0.1N NaOH; 50°C) have not made any significant changes in both BEN and MET but peroxide (3% H2O2; 28°C) have degraded the BEN but MET was unaffected. Conclusion: The present SCX method represented the shortest run time for the investigation of benidipine and metoprolol where the results of linearity, accuracy, precision, robustness and specificity were under the obligation of ICH guidelines.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"9 1","pages":"06-12"},"PeriodicalIF":0.0,"publicationDate":"2020-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80489532","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

A Novel Rapid Approach for the Estimation of Ketoconazole Using Reverse Phase Ultra Performance Liquid Chromatography in Bulk and Tablet Dosage from 反相超高效液相色谱法快速测定中药中酮康唑的原料药和片剂用量

Pharmaceutical Methods Pub Date : 2020-09-25 DOI: 10.5530/PHM.2020.1.1

S. Mondal, C. Alekya, P. Mondal

引用次数: 1

RP-HPLC and Spectrophotometric determination of rutin Trihydrate, Berberine chloride and trigonelline Hydrochloride in Antidiabetic Polyherbal Formulations 反相高效液相色谱法和分光光度法测定抗糖尿病复方制剂中三水芦丁、氯化小檗碱和盐酸葫芦巴碱的含量

Pharmaceutical Methods Pub Date : 2020-07-28 DOI: 10.5958/0974-360x.2020.00584.3

P. Chaudhary, Harsha U. Patel

引用次数: 4

New Stability Indicating LC Method for Novel Antidiabetic Drug Canagliflozin Hemihydrate Quantification; Development and Validation 新型降糖药半水合卡格列净定量稳定性指示LC法开发和验证

Pharmaceutical Methods Pub Date : 2019-09-19 DOI: 10.5530/PHM.2019.2.11

Satheesha Babu Birur Kotappa, R. Bhatta, Sadashivaiah Rudragangaiah

{"title":"New Stability Indicating LC Method for Novel Antidiabetic Drug Canagliflozin Hemihydrate Quantification; Development and Validation","authors":"Satheesha Babu Birur Kotappa, R. Bhatta, Sadashivaiah Rudragangaiah","doi":"10.5530/PHM.2019.2.11","DOIUrl":"https://doi.org/10.5530/PHM.2019.2.11","url":null,"abstract":"Introduction: The present research includes a new RP-HPLC method development and validation of Canagliflozin Hemihydrate (CANAG) a novel antidiabetic drug. The novel analytical method developed was employed for the quantification of CANAG in bulk drug and as an Active Pharmaceutical Ingredient (API) in tablet formulation. Methods: The present study utilized HPLC instrument (Shimadzu) comprises of ultraviolet detector and COSMICSIL 100 C18 (250 × 4.6 mm) 5 μm column. The mobile phase consists of acetonitrile: water (70:30%v/v) of pH 3.0±0.05 adjusted by addition of ortho-phosphoric acid. The chromatographic conditions were, flow rate 1 ml/min, run time 6.0 min, injection volume 20 μl and detection wavelength 282 nm at room temperature. The developed method was validated as per International Conference on Harmonization (ICH) guidelines for achieving robustness and accuracy. Forced degradation studies were carried out to prove the capability of the developed method to quantify the CANAG analyte response in presence of degraded products. Results: The presently developed novel analytical method possesses a shorter retention time 4.1 min. The results of validation parameters suggested that the presently developed method was robust and accurate since %RSD, theoretical plates and tailing factor values were within the limits of ICH guidelines. The predominant principle peak was observed in the chromatogram for CANAG without any interference from peaks of the degraded products. Conclusion: The present research study concluded that the developed analytical method for CANAG was novel, robust accurate and the principle peak of CANAG was not affected by presence of degraded and products. The same method can be employed for analysis of CANAG as a bulk drug and as API in formulation.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"199 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74977296","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: 0

Physicochemical and Phytochemical Analysis of Different Plant Parts of Annona muricata L. (Annonaceae) 番荔枝科番荔枝不同部位的理化及植物化学分析

Pharmaceutical Methods Pub Date : 2019-09-19 DOI: 10.5530/PHM.2019.2.13

Aditi Venkatesh Naik, K. Sellappan

{"title":"Physicochemical and Phytochemical Analysis of Different Plant Parts of Annona muricata L. (Annonaceae)","authors":"Aditi Venkatesh Naik, K. Sellappan","doi":"10.5530/PHM.2019.2.13","DOIUrl":"https://doi.org/10.5530/PHM.2019.2.13","url":null,"abstract":"Background: Annona muricata L. possesses multitudinous curative benefits and used traditionally to treat diverse ailments including cancer. The current study was undertaken to assess and investigate the physicochemical and phytochemical profile in different parts (rind, pulp, seed, leaf, bark and root) of Annona muricata L. collected from the State of Goa to determine requisite pharmacognostic standards for evaluating the plant material. Methods: Comparative assessment of physico-chemical parameters of plant parts viz. moisture loss, total ash, water soluble ash, acid insoluble ash and extractives were determined according to WHO recommended parameters for standardization. Phytochemical analysis to evaluate the effect of extractive solvents to determine difference of solvent polarity to phytochemical content, using aqueous, methanol, ethanol, ethyl acetate, chloroform, petroleum ether and hexane as solvents. Results: Physicochemical parameters revealed constants for identification and authentication of plant parts of A. muricata. Phytochemical analysis manifested the presence of salient classes of phytoconstituents. Among the solvents used for extraction, methanol showed the maximum yield of extract for all plant parts. Interestingly, major phytochemicals has polar properties largely extracted by methanol and part of them had semi-polar properties extracted by other polar and semi-polar solvents including alkaloids, flavonoid, saponin, phenol, tannin, proteins, amino acids, quinones and reducing sugars. Phytosterols, coumarins, fixed oils and fats were largely detected in non-polar solvents such as chloroform, petroleum ether and hexane. Conclusion: The findings of the present study form referential data for identification and standardization of the plant material for pharmaceutical applications.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"232 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75608779","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: 14

Novel Stability Indicating RP-HPLC Coupled with PDA Detection for the Simultaneous Quantification of Artesunate and Amodiaquine in Bulk and its Tablet 新型稳定性指示反相高效液相色谱- PDA检测同时测定散装及片剂中青蒿琥酯和阿莫地喹的含量

Pharmaceutical Methods Pub Date : 2019-09-19 DOI: 10.5530/phm.2019.2.12

P. Mondal, Devarakonda Krishnaprasad, Anusha Kusuma, Megha N Kulkarni, M. S. Reddy, Venu Kola, Padmaja Bookya

{"title":"Novel Stability Indicating RP-HPLC Coupled with PDA Detection for the Simultaneous Quantification of Artesunate and Amodiaquine in Bulk and its Tablet","authors":"P. Mondal, Devarakonda Krishnaprasad, Anusha Kusuma, Megha N Kulkarni, M. S. Reddy, Venu Kola, Padmaja Bookya","doi":"10.5530/phm.2019.2.12","DOIUrl":"https://doi.org/10.5530/phm.2019.2.12","url":null,"abstract":"Background: The present research paper reports the development of novel, stable and validated RP HPLC method for the simultaneous estimation of Artesunate (ATS) and Amodiaquine (AMDQ) in bulk and tablet dosage form. Methods: Good chromatographic separation was achieved by isocratic mode with a mixture of Phosphate Buffer: Methanol in the ratio of 60: 40 as mobile phase with waters symmetry Shield Rp18Column (250 mm x 4.6mm) and 5 micron particle size as stationary phase at flow rate of 1.0 mL/min. The detection was performed at 223 nm. Retention times for ATS and AMDQ were found 3.6 and 1.5 min respectively. Results: The proposed method showed good intra-day precisions (%RSD=0.36 for ATS, 0.50 for AMDQ), highly accurate (recovery for both ATS and AMDQ>99%) and satisfactory correlation coefficient (R2= 0.9914 for ATS and 99.38 for AMDQ). The detection and Quantitation limit were 0.53 μg/mL and 0.48 μg/mL for ATS, 1.23 μg/mL and 1.78 μg/mL for AMDQ. The percentage recovery in forced degradation study using acid, base, oxidation, photolytic, thermal and neutral conditions shows satisfactory and indicates well separation of both the drugs with other degradation products and the developed method also found good solution stability. Conclusion: Therefore, the present method was found stability indicating untroubled method ever developed, useful for the routine analysis of both the mentioned drugs in bulk as well as tablet dosage form.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"27 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82458490","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

Estimation of Eravacycline Dihydrochloride in Biological Matrices by LC-MS/MS LC-MS/MS法测定生物基质中盐酸依拉瓦环素的含量

Pharmaceutical Methods Pub Date : 2019-09-19 DOI: 10.5530/PHM.2019.2.9

B. S. Prasad, Sekharan Jaya Kumari

引用次数: 1

A New Stability Indicating High Performance Liquid Chromatography Method for the Estimation of Ruxolitinib in Bulk and Tablet Dosage Form 一种新的稳定性指示高效液相色谱法测定鲁索利替尼散装和片剂的含量

Pharmaceutical Methods Pub Date : 2019-09-19 DOI: 10.5530/PHM.2019.2.10

S. Biswal, S. Mondal, P. Mondal

{"title":"A New Stability Indicating High Performance Liquid Chromatography Method for the Estimation of Ruxolitinib in Bulk and Tablet Dosage Form","authors":"S. Biswal, S. Mondal, P. Mondal","doi":"10.5530/PHM.2019.2.10","DOIUrl":"https://doi.org/10.5530/PHM.2019.2.10","url":null,"abstract":"Background: The present research work described about the systemic development of High-Performance Liquid Chromatography (HPLC) method for the quantitative determination of ruxolitinib in bulk and tablet dosage form. The subsequent validation and degradation study was also performed. Methods: The chromatographic Separation was achieved with a HPLC (Waters-717 series) Symmetry ODS RP C18, 250mm x 4.6mm.i.d., 5μm,column with an isocratic mobile phase containing a mixture of acetonitrile: methanol: 1% Ortho phosphoric acid in the volume ratio of 70:25:5. The flow rate of the mobile phase was 1 ml/min and detection wavelength at 258 nm. The developed method was validated according to the ICH guidelines with respect to linearity, accuracy, precision, specificity, detection limits and robustness. Results: The precision of the results, stated as the %RSD was below 1.0%. The accuracy of the method demonstrated at three levels in the range of 50%, 100% and 150% of the specification limit. The calibration curve was linear over a concentration range from 5 to 200μg/ml with a correlation coefficient of 0.9997. The recovery of ruxolitinib was found to be in the range of 98 to 101%, whereas the detection limits were found to be 0.09 and quantitation limit was 0.29 μg/ml. Forced degradation study reveals its higher degradation at thermal and peroxide conditions in compare to other degradation condition. Conclusion: The present method was validated according to the ICH guidelines and it is applied successfully for the determination of ruxolitinib in tablets.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"13 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90860887","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: 7