{"title":"Development and Validation of a SPE-HPLC Method for Quantification of Rhein, Emodin, Chrysophanol and Physcion in Rhamnus petiolaris Boiss. & Balansa.","authors":"Pelin Köseoğlu Yılmaz, Ufuk Kolak","doi":"10.1093/chromsci/bmad053","DOIUrl":"10.1093/chromsci/bmad053","url":null,"abstract":"<p><p>Anthraquinones exhibit a significant group of natural and synthetic quinone derivatives because of their biological activities and industrial applications. Rhamnaceae is one of the families known to contain different kinds of anthraquinones. In this study, it was aimed to quantify rhein, emodin, chrysophanol and physcion in fruits of Rhamnus petiolaris Boiss. & Balansa belonging to Rhamnaceae by solid phase extraction and high performance liquid chromatography with ultraviolet detection. The anthraquinones were separated using a C18 analytical column. Gradient elution was performed using a mobile phase consisted of 0.1% o-phosphoric acid solution and methanol. Analytes were detected at 254 nm. Calibration curves were prepared in the range of 0.25-5.00 μg/mL for rhein, chrysophanol, physcion, 1.00-50.00 μg/mL for emodin. Limits of detection and quantification were between 0.07-0.11 and 0.20-0.34 μg/mL, respectively. Relative standard deviations were ≤ 5.78% in repeatability and intermediate precision studies. Accuracy was determined as relative mean error (8.17-12.06%). Extraction was achieved by maceration with acetone and ethanol, followed by hydrophilic-lipophilic balance solid phase extraction. Recoveries were between 96.2 and 109.6%. The developed and validated method was successfully performed to quantify rhein, emodin, chrysophanol and physcion in R. petiolaris fruit extracts. Only physcion was not detected above limit of detection.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"872-877"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11530379/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10259909","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Development and Validation of a Simple High-Pressure Liquid Chromatography-Ultraviolet Detection Method for Simultaneous Quantitation of First-Line Anti-Tuberculosis Drugs in Formulations of Fixed-Dose Combination.","authors":"Sudha Vilvamani, Santhanamahalingam Mahalingam, Sruthi Nhavilthodi, Dharman Murugesan, Shanmugam Murugaiha Jeyakumar","doi":"10.1093/chromsci/bmae023","DOIUrl":"10.1093/chromsci/bmae023","url":null,"abstract":"<p><p>The current treatment protocol for drug-sensitive tuberculosis involves all four first-line anti-tuberculosis drugs: rifampicin, isoniazid, pyrazinamide and ethambutol hydrochloride in a single tablet, known as fixed-dose combination tablets. However, the analytical methods are scanty to test all these drugs simultaneously in a single run without any pre-sample process or using a simple method suitable for resource-limited settings. In this method, 50 mM potassium phosphate buffer containing 0.2% triethylamine (without pH adjustment) added with acetonitrile (98:2, v/v) was served as mobile phase A, while mobile phase B was 100% acetonitrile. All four drugs were separated within 10.3 min using a gradient mobile phase program in a C18 column (150 mm × 4.6 mm; 5 μm) and detected at two ultraviolet wavelengths (238 nm for rifampicin, isoniazid and pyrazinamide, and 210 nm for ethambutol hydrochloride). The method was selective, sensitive and linear with a correlation coefficient >0.999 with the acceptable precision and accuracy (<2% relative standard deviation) for all four drugs. In conclusion, the method is simple and it does not require any pH adjustment of the buffer/mobile phase, and within 11 min, the separation of all four drugs can be achieved. Overall, the method is suitable for quality testing of fixed-dose combination tablets in limited-resource settings.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"821-828"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140876568","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Xiaoli Xu, Lin Yang, Dezhang Zhao, Yiwu Wang, Lei Dai, Shuya Li, Dan He
{"title":"New Quality Evaluation of Qizhi Xiangfu Pills Based on Fingerprint with Chemometric Analysis and Quantitative Analysis of Multi-Components by Single Marker.","authors":"Xiaoli Xu, Lin Yang, Dezhang Zhao, Yiwu Wang, Lei Dai, Shuya Li, Dan He","doi":"10.1093/chromsci/bmae005","DOIUrl":"10.1093/chromsci/bmae005","url":null,"abstract":"<p><p>Qizhi Xiangfu Pills (QZXFPs) is one of the most commonly used traditional Chinese medicine preparations for the treatment of dysmenorrhea, but the existing quality evaluation standards have certain shortcomings and deficiencies. An effective and scientific quality evaluation method plays a vital role in medication safety. In this study, fingerprint combined with chemometric analysis and quantitative analysis of multi-components by a single marker (QAMS) method was used to comprehensively evaluate the quality of QZXFPs. The fingerprints of 28 batches samples were established and 23 common peaks were distinguished, of which 7 peaks were identified as albiflorin, paeoniflorin, baicalin, ligustilide, cyperotundone, nootkatone and α-cyperone. The content of these seven active ingredients was determined simultaneously by the QAMS method and there was no significantly different between QAMS and the external standard method. Additionally, similarity analysis, hierarchical cluster analysis, principal component analysis and orthogonal partial least squares discrimination analysis were applied for classifying the 28 batches of samples, and to find the main components causing the quality differences between different batches. In conclusion, the established method can comprehensively evaluate the consistency of quality between different batches and provide a reference for formulation quality evaluation to ensure safe and effective application of QZXFPs.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"854-863"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140049658","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Thiazolidinediones: Recent Development in Analytical Methodologies.","authors":"Tarang Patel, Vatsal Patel","doi":"10.1093/chromsci/bmad058","DOIUrl":"10.1093/chromsci/bmad058","url":null,"abstract":"<p><p>The instrumental analytical methods that have been developed and utilized for the determination of thiazolidinedione in bulk medications, formulations and biological fluids have been reviewed after an in-depth analysis of the literature published in a variety of analytical and pharmaceutical chemistry-related journals. The approaches covered by this research, which covers the years 2001-2022, include complex methods for analysis, chromatographic techniques and spectrometric analytical procedures. The mobile phase, flow rate, sample matrix, wavelength and other factors identified in the literature were just a few of the parameters used to evaluate thiazolidinediones. The present review focuses on the published analytical techniques for thiazolidinedione analysis that have been previously identified in the literature. The specified outcomes followed extensive learning, and the most recent advances in analytical methods for the identification of pioglitazone, pioglitazone HCl, rosiglitazone, rosiglitazone maleate and lobeglitazone were reviewed. Additionally, this article briefly discusses features of analytical discovery on thiazolidinediones, which will enable readers to access all discoveries in one place with precise outcomes.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"789-802"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10274299","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Correction to: Thiazolidinediones: Recent Development in Analytical Methodologies.","authors":"","doi":"10.1093/chromsci/bmad080","DOIUrl":"10.1093/chromsci/bmad080","url":null,"abstract":"","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"804"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10291357","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Correction to: Solid-Phase Extraction (SPE) Technique to Quantify Cefdinir in Human Plasma Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS).","authors":"","doi":"10.1093/chromsci/bmad044","DOIUrl":"10.1093/chromsci/bmad044","url":null,"abstract":"","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"803"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9640000","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Novel RP-HPLC Method for Simultaneous Estimation of Vilanterol Trifenatate, Umeclidinium Bromide and Fluticasone Furoate in Inhalation Dry Powder Formulation.","authors":"Shweta Yadav, Vandana Jain, Hemant Magar, M Vijay Kumar, Sayali Warde, Raman Mohan Singh","doi":"10.1093/chromsci/bmad075","DOIUrl":"10.1093/chromsci/bmad075","url":null,"abstract":"<p><p>The dry powder inhalation formulation containing vilanterol trifenatate, umeclidinium bromide and fluticasone furoate intended for the therapy of bronchospasm related to chronic obstructive pulmonary disease and bronchial asthma was selected for the development and validation of a novel, selective, accurate, precise, quick and cost-efficient reversed-phase, high-performance liquid chromatography method. Neither an official monograph nor a single method has yet been published for the simultaneous estimation of these three compounds, which makes this method novel. The stationary phase of an ACE-C18-PFP column (250 mm × 4.6 mm, 5 μ) was used with a mobile phase of 25-mM sodium perchlorate buffer (pH 2.5 adjusted with ortho-phosphoric acid) and acetonitrile (40:60% v/v) at a flow rate of 1 mL/min to optimize chromatographic variables. The column temperature was kept at 40°C, and detection was at 224 nm, which was the isosbestic point of these three drugs. Well-resolved good peak symmetry was obtained for all three molecules by isocratic elution in less than 10 min, and the retention times of vilanterol trifenatate, umeclidinium bromide and fluticasone furoate were found to be 3.7, 5.4 and 8.3 min, respectively. The proposed method was validated as per ICH Q2 (R1) guidelines, and the calibration curves were linear in concentration ranges of 5-35 μg/mL for vilanterol trifenatate, 5-80 μg/mL for umeclidinium bromide and 5-150 μg/mL for fluticasone furoate, with mean % recoveries of 99-100%. The limits of detection and quantitation are 0.15 and 0.45 μg/mL for vilanterol trifenatate, 0.58 and 1.77 μg/mL for umeclidinium bromide and 0.32 and 0.96 μg/mL for fluticasone furoate, respectively. Hence, the proposed RP-HPLC technique was successfully used to quantify the inhalation formulation containing all three compounds.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"761-766"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10172968","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"UPLC-PDA Approach for Simultaneous Quantification of Elvitegravir, Tenofovir, Emtricitabine and Cobicistat in Tablets: An MS-ESI Study for Degradation Products.","authors":"Rajya Lakshmi Nimmagadda, Sowjanya Gummadi","doi":"10.1093/chromsci/bmad067","DOIUrl":"10.1093/chromsci/bmad067","url":null,"abstract":"<p><p>A simultaneous ultra-performance liquid chromatography photodiode array detection method was developed and validated for Elvitegravir, Tenofovir and Emtricitabine and Cobicistat drugs in tablet dosage forms. Effective liquid chromatographic quantification was achieved using a Luna C18 (100 × 2.6 mm, 1.6 μ) column with an acetonitrile: 0.1% v/v trifluoro acetic acid (80:20% v/v) mobile phase and a photo diode array detector at 260 nm for a shorter run time of 3 min. The respective retention times for Elvitegravir, Tenofovir, Emtricitabine and Cobicistat were 0.311, 0.792, 1.379 and 2.045 min. The range of linearity was 37.50-225.00, 2.50-15.00, 50.00-300.00 and 37.50-225.00 μg/mL for Elvitegravir, Tenofovir, Emtricitabine and Cobicistat, respectively. A mass spectrometer was employed for quantitative analysis using electron spray ionization multiple reaction monitoring in positive mode. The developed method was validated for different parameters to meet the acceptance criteria as per ICH Q2 (R1) guidelines. Using UPLC-ESI-MS, 12 degradants were identified and their mechanisms were studied.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"719-731"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10257145","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Tarun Shishodia, Parul Grover, K Nagarajan, Monika Bhardwaj, Bhawna Chopra
{"title":"Development and Validation of Robust, Highly Sensitive and Stability-Indicating RP-HPLC Method for Estimation of Deferasirox and its Degradation Products.","authors":"Tarun Shishodia, Parul Grover, K Nagarajan, Monika Bhardwaj, Bhawna Chopra","doi":"10.1093/chromsci/bmad032","DOIUrl":"10.1093/chromsci/bmad032","url":null,"abstract":"<p><p>A rapid, simple and highly sensitive stability-indicating reverse-phase high-performance liquid chromatographic technique, coupled with a photodiode array detector, was developed and validated for the estimation of Deferasirox (DFS). The chromatographic separation was achieved using a C-18 (250 × 4.6 mm, 5 μm) stationary phase and a mobile phase composed of 0.1% orthophosphoric acid and acetonitrile at a flow rate of 1 mL/min. The detection was carried out at a wavelength of 245 nm with a constant injection volume of 10 μL throughout the analysis. With an R2 value of 0.9996, the calibration curve was determined to be linear over an appropriate concentration range of 50-500 ng/mL. According to the International Conference on Harmonization (ICH) Q1 (R2) guideline, DFS was evaluated under stress conditions that included hydrolytic (acid, alkali and neutral), oxidative and thermal degradation. The findings demonstrated that significant degradation was observed in acidic degradation conditions, whereas drug substance was found to be stable when exposed to neutral, basic, oxidative and thermal degradation. The developed method was validated as per ICH guidelines. The developed method was employed successfully to estimate the amount of DFS in bulk and pharmaceutical formulation.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"709-718"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9687991","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Foram Patel, Rajendra Kotadiya, Rashmin Patel, Mrunali Patel
{"title":"Development and Validation of a New Reversed Phase HPLC Method for the Quantitation of Azithromycin and Rifampicin in a Capsule Formulation.","authors":"Foram Patel, Rajendra Kotadiya, Rashmin Patel, Mrunali Patel","doi":"10.1093/chromsci/bmae006","DOIUrl":"10.1093/chromsci/bmae006","url":null,"abstract":"<p><p>This research aimed to develop a new method for simultaneously estimating the presence of azithromycin (AZT) and rifampicin (RIF) in a capsule formulation using reverse-phase high-performance liquid chromatography. The developed method utilized a Gemini column with a 60:40% v/v acetonitrile and potassium dihydrogen phosphate mobile phase, a flow rate of 1 mL/min, and an injection volume of 20 μL. The detection wavelengths of 210 and 254 nm for AZT and RIF, respectively, were used. Validation ensures specificity with a peak purity index > 0.99999 for AZT and >0.99995 for RIF, affirming unambiguous analyte detection. The system suitability test, within acceptable limits, validates method reliability. Linearity calibration curves (R2 = 0.998) cover a 25-150% target concentration range. Accuracy studies employing the standard addition method yield recovery values between 96.6 and 103.9% for both drugs, confirming method accuracy. Precision studies reveal % relative standard deviation values consistently below 2%, highlighting reproducibility. Robustness testing supports method reliability under varying conditions. Application to a pharmaceutical capsule formulation demonstrates the method's practicality, accurately quantifying AZT (98.30%) and RIF (99.37%). This study provides a validated analytical approach for simultaneous quantification in commercial pharmaceutical products containing both drugs, enhancing pharmaceutical quality control for critical antibiotics in complex formulations.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"742-750"},"PeriodicalIF":1.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140140324","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}