{"title":"Glycopyrronium bromide, formoterol fumarate dihydrate and their related compounds with UPLC/PDA-MS for simultaneous determination in pressurized metered-dose inhaler product.","authors":"Serdar Seckin, Serap Saglik Aslan","doi":"10.1093/chromsci/bmag030","DOIUrl":"10.1093/chromsci/bmag030","url":null,"abstract":"<p><p>An ultra-performance liquid chromatography (UPLC) technique with photodiode array-mass spectrometry (PDA-MS) detectors has been developed and validated for the determination of glycopyrronium bromide (GB), formoterol fumarate dihydrate (FFD) and their related substances in pressurized meter dose inhalers. This marks the first time the method has been implemented. Chromatographic analyses have been carried out on a UPLC system with a single quadrupole mass spectrometer (QDa) and a PDA detector. A C18 column has been used prior to the injection valve. The column temperature was set to 40°C. For each analysis, 1 μL of sample was injected at a flow rate of 0.1 mL/minute. The mobile phases used were A (0.5% formic acid in methanol) and B (0.5% formic acid in water). The total run time of the method was 30 minutes. The PDA detector was employed at 215 nm while the mass detector was set to extracted ion chromatography (XIC) mode. The range for detecting impurities of GB was found to be between 0.28 and 0.30 ng/mL, with a limits of 0.92-1.01 ng/mL for quantification. GB and FFD demonstrated linear accuracy. We studied the accuracy of related substances within the limit of quantification value range of corresponding impurities and up to 400% of the limit value. The method we used was linear, rapid, reproducible and accurate. Our proposed method is fast, linear, accurate and reproducible. The UPLC-MS method, which utilized QDa with XIC mode, was developed to ascertain the related substances and assay of GB and FFD.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13677063/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149220177","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":"Correction to: Plain and Ion-Pair Thin-Layer Chromatography of Synthetic Dyes on an Admixture of Silica Gel G and Barium Sulfate in an Aqueous Ethanol System.","authors":"","doi":"10.1093/chromsci/bmag031","DOIUrl":"https://doi.org/10.1093/chromsci/bmag031","url":null,"abstract":"","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149171523","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":"In memoriam: Professor Huba Kalász (1941 - 2026).","authors":"Ernest A Adeghate","doi":"10.1093/chromsci/bmag029","DOIUrl":"https://doi.org/10.1093/chromsci/bmag029","url":null,"abstract":"","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 9","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-10-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149166122","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":"Rapid and validated LC-APCI-MS/MS method for determination of N-nitroso vonoprazan in pharmaceutical products.","authors":"Filiz Demir, Sıdıka Ertürk Toker","doi":"10.1093/chromsci/bmag024","DOIUrl":"https://doi.org/10.1093/chromsci/bmag024","url":null,"abstract":"<p><p>The primary objective of this study was to develop and validate a liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometric (LC-APCI-MS/MS) method for the determination of trace levels of N-nitroso vonoprazan (NVNP) in vonoprazan active pharmaceutical ingredient (API) and pharmaceutical products. Chromatographic separation was achieved on an Acquity® Premier HSS T3 column under isocratic conditions using 0.1% formic acid in water and acetonitrile as the mobile phase. Detection was performed in positive ion mode using multiple reaction monitoring. The method was validated according to ICH Q2(R2) guidelines for selectivity, linearity, accuracy, precision, robustness, matrix effect, limit of detection (LOD), and limit of quantification (LOQ). The method was linear over the concentration range of 0.24-50.0 ng/mL (R2 = 0.9971), with recoveries of 85.6%-99.2% and relative standard deviation values below 6.1%. The validated LOD and LOQ were 0.10 and 0.24 ng/mL, respectively; the latter corresponds to 0.24 μg/g (240 ppb) in the pharmaceutical product. Matrix effect evaluation showed 91.6% response (8.4% ion suppression), indicating minimal matrix interference. The validated LC-APCI-MS/MS method was successfully applied to both API and finished products and is suitable for routine quality control, stability studies, nitrosamine risk assessment, and regulatory monitoring of NVNP.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148864966","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}
Haitham A El Fiky, Maha F Abd El Ghany, Amr M Badawey, Nermine V Fares, Dina A Ahmed
{"title":"Eco-friendly stability-indicating chromatographic methods with integrated molecular docking and ADMET evaluation for simultaneous determination of carvedilol and ivabradine.","authors":"Haitham A El Fiky, Maha F Abd El Ghany, Amr M Badawey, Nermine V Fares, Dina A Ahmed","doi":"10.1093/chromsci/bmag028","DOIUrl":"https://doi.org/10.1093/chromsci/bmag028","url":null,"abstract":"<p><p>Currently, many researchers strive to create eco-conscious methods for drug separation to avoid hazardous solvents. In line with this objective, this study focuses on developing two green chromatographic methods, TLC and UPLC, to determine the mixture of carvedilol (CAR) and ivabradine (IVA) used for controlling stable angina symptoms, along with their oxidative degradates. The TLC method employed toluene: methanol: ammonia (8:2:0.2, by volume) as a mobile phase and silica gel plates as the stationary phase, with detection at 270.0 nm using concentration ranges of 0.5-8.0 μg/band for each drug. The optimized UPLC method utilized a mobile phase of ethanol: 0.1% triethylamine adjusted by acetic acid to pH 6.4 (40:60 v/v) on an Agilent Poroshell C18 (150 mm × 3 mm) column, with a 0.3 mL/min flow rate at 30°C and fluorimetric detection at 285.0 nm excitation and 330.0 nm emission, with linearity of 0.2-12.0 μg/mL for both drugs. Green assessment of the proposed methods with 82 and 78 green Eco-scores, AGREE score values of 0.77 and 0.72 for UPLC and TLC methods, respectively were performed. Moreover, statistical comparison of the proposed methods with reported and official methods was conducted. Additionally, structure elucidation, molecular docking and ADMET assessment of the degradates were successfully performed.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149024987","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":"QbD consideration for developing and validating the dissolution test method for quantitative analysis of tadalafil chewable tablets.","authors":"Seung-Hyun Park, Joo-Eun Kim","doi":"10.1093/chromsci/bmag025","DOIUrl":"https://doi.org/10.1093/chromsci/bmag025","url":null,"abstract":"<p><p>Erectile dysfunction (ED) is defined as the persistent inability to achieve or maintain an erection sufficient for satisfactory performance for a duration of >3 months. However, chewable tadalafil formulations for treating ED and corresponding dissolution analysis methods for their quantification are lacking. Therefore, this study aims to investigate Quality by Design considerations for developing a reversed-phase high-performance liquid chromatography method. The test method was designed to perform a quantitative dissolution analysis of tadalafil chewable tablets to enhance medication compliance. This method required an Agilent C8 column (4.6 × 5.0 cm, 5 μm) as the stationary phase and a mobile phase comprising a 1:1 methanol-water mixture. The column temperature and detection wavelength were maintained at 40°C and 225 nm, respectively. The development and validation of the dissolution method resulted in a relative standard deviation of 0.03% for system suitability, assessed in a test solution containing a solubilizer. The test method demonstrated specificity by clearly distinguishing the active pharmaceutical ingredient from excipients. Tadalafil accuracy was confirmed with an average recovery rate of 100.22%, and the precision showed a relative standard deviation of 0.35%. Excellent linearity (R2 = 1.000) was observed over the concentration range of 1.5 μg/mL to 9.0 μg/mL. Additionally, the detection and quantification limits for tadalafil were 0.003 μg/mL and 0.008 μg/mL, respectively. The developed method facilitated rapid quantification of tadalafil in chewable tablets, completing each run within 5 min and reducing analysis time by ~60% compared to conventional methods. Additionally, reagent consumption and operational costs were reduced by ~45%, improving overall efficiency. These findings validate the suitability of the method for reliable industrial quality control of tadalafil chewable tablets and new formulations.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148891741","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":"Analysis of principal components and fragmentation patterns of Tinosporae Radix by ultra high-performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry.","authors":"Dianchao Tang, Chen Jin, Yiling Yang, Zexi Wang, Lanlan Zhong, Zhongwan Yang, Hui-Lian Huang","doi":"10.1093/chromsci/bmag027","DOIUrl":"https://doi.org/10.1093/chromsci/bmag027","url":null,"abstract":"<p><p>In this study, ultra high-performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry was employed to characterize and identify the chemical constituents in the total extract of Tinosporae Radix. Chromatographic separation of the total extract was carried out on a Waters chromatographic column (100 mm × 2.1 mm, 1.7 μm) with a gradient elution program using a mobile phase system consisting of 0.1% aqueous formic acid (v/v, solvent A) and acetonitrile (solvent B). Mass spectrometric detection was conducted in both positive and negative ion modes. A total of 43 chemical components were successfully identified, including 29 alkaloids and 14 terpenoids. Furthermore, the mass fragmentation behaviors and characteristic fragment ions of protoberberine isoquinoline alkaloids, aporphine alkaloids and diterpenes were systematically analyzed. This study provides reliable reference data for the identification and compositional analysis of chemical constituents in Tinosporae Radix and its homologous medicinal herbs. The findings lay a solid foundation for exploring the pharmacodynamic material basis and chemical profiling of this traditional Chinese medicinal herb, supporting its quality evaluation and further pharmacological mechanism research.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149016987","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}
Julia Cavalcante Faria, Vítor Todeschini, Maximiliano da Silva Sangoi
{"title":"Rapid quantitative determination of zidovudine, lamivudine and nevirapine drugs in pharmaceutical tablets by stability-indicating monolithic liquid chromatography: validation, greenness, blueness and whiteness studies.","authors":"Julia Cavalcante Faria, Vítor Todeschini, Maximiliano da Silva Sangoi","doi":"10.1093/chromsci/bmag026","DOIUrl":"https://doi.org/10.1093/chromsci/bmag026","url":null,"abstract":"<p><p>New ecological, sustainability and practicality analytical methodologies became constant in the modern pharmaceutical analysis. Likewise, a simple, rapid, stability-indicating high-performance liquid chromatography (HPLC) method was developed and validated for simultaneous determination of lamivudine (3TC), zidovudine (ZDV) and nevirapine (NVP) in pharmaceutical formulations. The HPLC method was carried out on a monolithic C18 column (100 mm × 4.6 mm i.d.), maintained at 30°C. The mobile-phase consisted of ammonium acetate (pH 4.5; 10 mM)-methanol-acetonitrile (65:28:7, v/v/v), run at a flow rate of 2.0 mL/min, using photodiode array (PDA) detection at 270 nm. Validation parameters such as the specificity, linearity, precision, accuracy and robustness were evaluated according to the International Council for Harmonisation (ICH) guidelines. From the results obtained, the developed HPLC method was successfully applied for the simultaneous quantitative analysis of 3TC, ZDV and NVP in tablet dosage forms. The chromatographic separation was obtained in less than 3 min and it was suitable for high-throughput analysis. In addition, the greenness assessment, the holistic overall evaluation and the practicality check using the novel Analytical GREEnness Metric Approach and Software (AGREE) calculator, the RGB-12 model and Blue Applicability Grade Index (BAGI), respectively, were performed. The results demonstrated the environmental friendliness (AGREE), practicality (BAGI) and holistic sustainability profile (RGB-12 model) of the proposed method.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149016952","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":"\"Simultaneous quantification of nystatin, triamcinolone acetonide, neomycin sulfate and gramicidin D in transferosomal gel by rapid stability indicating HPLC method with PDA detector\".","authors":"Sasikala Allam, Annammadevi G S, Gowri Gollu, Sandeepchary Padakanti, Nalini Mathala, Lekhya Gurijala, Deepthi Vemuri, Janardhan Swamy Adabala","doi":"10.1093/chromsci/bmag016","DOIUrl":"https://doi.org/10.1093/chromsci/bmag016","url":null,"abstract":"<p><p>The present study aimed to develop and validate a simple, rapid and stability-indicating high-performance liquid chromatographic (HPLC) method for the simultaneous quantification of nystatin (Nys), neomycin sulfate (NS), triamcinolone acetonide (TAC) and gramicidin D (Gr) in bulk drug samples and transferosomal gel formulations. Chromatographic separation was achieved on an Agilent Eclipse C18 (250 × 4.6 mm, 5 μm) using a mobile consisting of methanol and 0.1% orthophosphoric acid (30:70, v/v). The flow rate was maintained at 1.0 mL/min, and detection was carried out at 260 nm using a Photo Diode Analyzer (PDA) detector. Under the optimized chromatographic conditions, all four analytes were eluted with symmetrical peaks, satisfactory resolution and acceptable theoretical plate counts within a run time of 12 min. The method exhibited excellent linearity over concentration ranges of 25-150 μg/mL for TAC, 62.5-375 μg/mL for Nys, 250-1,500 μg/mL for NS and 6.25-37.5 μg/mL for Gr, with correlation coefficients greater than 0.999 for all analytes. The developed method was validated according to International Council for Harmonization guidelines and demonstrated acceptable accuracy, with percentage recoveries ranging from 98 to 102% and precision, with percentage relative standard deviation values below 2%. Forced degradation studies were performed under acidic, alkaline, oxidative, reductive, thermal, photolytic, peroxide and hydrolytic conditions. The analytes exhibited degradation ranging from ~11 to 12.1%, confirming the stability-indicating capability of the method. The proposed method is simple, accurate, precise, robust and suitable for the routine quantification of Nys, NS, TAC and Gr in bulk drug substances, transferosomal gel formulations and marketed pharmaceutical products.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148912363","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}
Sathish Kumar Konidala, Srikar Grandhi, Harsha Sri Kamma
{"title":"Development of a stability-indicating RP-UPLC method for simultaneous determination of Abemaciclib and Olaparib with LC-MS characterization of degradation products and in vitro performance evaluation.","authors":"Sathish Kumar Konidala, Srikar Grandhi, Harsha Sri Kamma","doi":"10.1093/chromsci/bmag022","DOIUrl":"https://doi.org/10.1093/chromsci/bmag022","url":null,"abstract":"<p><p>The simultaneous determination of Abemaciclib and Olaparib in in-houseprepared tablets was accomplished by the development and validation of a novel and rapid and sensitive reverse-phase ultra-performance liquid chromatography (RP-UPLC) technique. Using a Waters X-Bridge C18 (4.6 × 100 mm, 3.5 μm) column and a mobile phase made up of 0.1% orthophosphoric acid in water, acetonitrile and methanol (70:20:10% v/v/v) in an isocratic elution mode at a flow rate of 1 mL/min, the chromatographic separation was accomplished. High sensitivity and selectivity were made possible by performing the detection at 219 nm. Following ICH Q2(R1) criteria, the technique was validated and showed high linearity (R2 > 0.999) for both drugs over the concentration range of 10-60 μg/mL. Within acceptable boundaries (<2% Relative Standard deviation (RSD)), both intra-day and inter-day precision and accuracy (recovery percentage) were proven. Forced degradation studies confirmed the method's stability-indicating capability, Stability studies indicated significant degradation under acid, alkali, peroxide and thermal degradation conditions. The degradation products were characterized by LC-MS technique, and possible degradation pathways were proposed. Additionally, in vitro pharmacokinetic evaluation, including dissolution and drug release kinetics, was performed to assess formulation performance. The developed method proved simple, precise and robust, making it suitable for routine quality control, stability study and pharmacokinetic studies of Abemaciclib and Olaparib co-formulated tablets.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 7","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148578731","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}