{"title":"Analytical quality by design (AQbD)-assisted bioanalytical method for the estimation of Lasmiditan in human plasma by reverse phase-high performance liquid chromatography (RP-HPLC).","authors":"Ajitha Azhakesan, Burugula Sparsha, Pasupuleti Kishore, Sujatha Kuppusamy","doi":"10.1093/chromsci/bmag012","DOIUrl":"10.1093/chromsci/bmag012","url":null,"abstract":"<p><p>Migraine is a complex neurological condition that often involves a severe headache characterized by moderate to severe throbbing. Lasmiditan a novel ditan approved by USFDA in 2011 to treat migraine. This contemporary research elaborates the systematic development and validation of Reverse Phase-High Performance Liquid Chromatography bio analytical method for estimating Lasmiditan in human plasma employing analytical quality by design. Bio analysis employing protein precipitation was performed to extract Lasmiditan from human plasma using Dolutegravir as the internal standard. Design of Experiments was incorporated employing central composite design, and the methodology was assessed for critical analytical attributes by varying the critical quality attributes using Design Expert Software Version 13.0. The chromatographic conditions optimized were symmetry C18 (150 × 4.6 mm, 5 μ) column, mobile phase 0.1% orthophosphoric acid: acetonitrile (70:30 (v/v) with a flow rate of 1.0 mL/min at detection wavelength of 260 nm and column temperature of 30°C. Validation studies indicated linearity between 20 and 800 ng/mL (r2 = 0.999), whereas accuracy and precision portrayed a 98.79% recovery. Succinctly, current work exemplifies the significant merits of analytical quality by design approach toward the holistic process in bioanalytical method validation. Furthermore, the method was evaluated using the Whiteness Assessment Tool (Blue Applicability Grade Index), yielding a high score of 82.5, indicating superior performance in terms of analytical efficiency, environmental friendliness and operator safety. Thus, the developed method can be applied for estimation of preclinical and clinical samples of Lasmiditan with improved accuracy and precision.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 4","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147673836","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":"Quantitative analysis of characteristic aroma components in rose hydrosol by reversed-phase liquid chromatography using hydroxypropyl-β-cyclodextrin as mobile-phase additive.","authors":"Wenli Zhang, Mengyi Wen, Junchao Zhu, Yuxia Chen, Wanghui Chen, Shengqiang Tong","doi":"10.1093/chromsci/bmag011","DOIUrl":"10.1093/chromsci/bmag011","url":null,"abstract":"<p><p>Quantitative determination of eight characteristic aroma components, namely, benzyl alcohol, phenylethyl alcohol, eugenol, geraniol, nerol, linalool, citronellol, and methyl eugenol, by reversed-phase high-performance liquid chromatography with hydroxypropyl-β-cyclodextrin as mobile-phase additive was investigated. The proposed method was validated and demonstrated with good linearity of 0.994 to 1.000 with a recovery in the range of 94.97-109.38% and exhibited favorable accuracy, intra and inter-day precision based on relative standard deviation values. Additionally, the inclusion complex between eight characteristic aroma components and hydroxypropyl-β-cyclodextrin was investigated, the complex formation was found at a 1:1 molal ratio for eight characteristic aroma components and hydroxypropyl-β-cyclodextrin, and the apparent formation constant between citronellol and hydroxypropyl-β-cyclodextrin was determined to be 71.86 M-1. In those components, ∆H of linalool and citronellol was found to be +877.03 kJ mol-1 and +1433.67 kJ mol-1, and ∆S were positive, which indicated that transfer from mobile phase to the stationary phase of the two analytes was entropically driven. Furthermore, this method was successfully applied to determination of characteristic aroma components in Rosa damascena Mill. hydrosol and R. rugosa cv. \"Plena\" hydrosol, in which it was found that phenylethyl alcohol, citronellol, and methyl eugenol were principal components.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 4","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147673814","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}
Ghanshyam B Paladiya, Jinal Tandel, Heta Kachhiya, Usmangani Chhalotiya, Dimal Shah, Devang Tandel
{"title":"Planer chromatographic method development and validation of Tadalafil and Mirabegron using fractional factorial design approach.","authors":"Ghanshyam B Paladiya, Jinal Tandel, Heta Kachhiya, Usmangani Chhalotiya, Dimal Shah, Devang Tandel","doi":"10.1093/chromsci/bmag014","DOIUrl":"10.1093/chromsci/bmag014","url":null,"abstract":"<p><p>The present research focuses on developing a high-performance thin-layer chromatographic (HPTLC) method using a design of experiment approach for simultaneously estimating Tadalafil and Mirabegron. Chromatographic separation was achieved on aluminum plates precoated with silica gel 60 F254 using an optimized mobile phase of MeOH: ACN: n-Butanol: TEA (6:2:2:0.1%v/v/v/v). A fractional factorial design was applied for the robustness study and the independent variables selected were chamber saturation time (A), wavelength (B), mobile phase composition (C) and solvent front (D). It was statistically revealed that the volume of MeOH affected the Rf of both drugs resulting in stricter control of MeOH volume compared to the other three variables. Rf for Tadalafil and Mirabegron was 0.75 and 0.45 at 242 nm. Calibration plots were linear for Tadalafil (100-300 ng/band) and Mirabegron (500-1500 ng/band), with recovery rates of 98.15%-100.34% and 98.46%-102.14%, respectively. The method was validated per ICH Q2(R1) guidelines, demonstrating linearity, precision, accuracy and selectivity, with %RSD values below 2% for both drugs. This HPTLC method is simple, accurate, reproducible and suitable for routine quality control of pharmaceutical formulations.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 4","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147772846","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":"Development and Validation of Reverse Phase High-Performance Liquid Chromatographic Method Enabling Simultaneous Estimation of Polmacoxib and its Process-Related Impurities: Exploring Degradation Pathways and Elucidating Degradant Structures via LC-MS/MS and NMR Spectroscopy.","authors":"Hitesh Thumbar, Bhavin Dhaduk","doi":"10.1093/chromsci/bmag006","DOIUrl":"10.1093/chromsci/bmag006","url":null,"abstract":"<p><p>A simple, sensitive, and selective reverse phase high-performance liquid chromatography (HPLC) method was developed and validated for the estimation of Polmacoxib (POL) and its process-related impurities. Chromatographic separation was achieved on a Kromasil C18 column (250 mm x 4.6 mm, 5 μm) using gradient elution with mobile phase containing 10 mM ammonium acetate buffer and acetonitrile in the initial ratio of 90:10 (% v/v). Chromatographic parameters were optimized: flow rate of 1.2 mL/min, UV detection at 232 nm, and injection volume of 10 μL. The developed method was validated as per International Council for Harmonization Q2 (R1) guidelines. For the stability study, the drug was subjected to various stress conditions. The results showed that was sensitive to the alkaline and degraded. Under alkaline condition, impurity-I and II were detected at retention time of 2.61 and 21.09 min, respectively. To identify the structures of the detected impurities, were initially isolated using a preparative HPLC and then collected fractions were injected into liquid chromatography with tandem mass spectrometry for structural identification. Further structure elucidation was performed using 1D-NMR (1H and 13C) and 2D-NMR (1H-1H correlation spectroscopy and 1H-13C heteronuclear single quantum coherence), and explore the degradation pathway. The proposed method is applicable for assay estimation of POL in dosage form and is suitable for quality control analysis.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147463232","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":"Fabrication of Trimetallic Metal-Organic Frameworks for the Rapid Removal of Bisphenol A from Water.","authors":"Rui Xu, Rui Xiao, Ming-Hua Lu","doi":"10.1093/chromsci/bmag003","DOIUrl":"https://doi.org/10.1093/chromsci/bmag003","url":null,"abstract":"<p><p>Metal-organic frameworks (MOFs) have attracted widespread attention owing to their promising applications in sample pretreatment. However, trimetallic MOFs remain a challenge to synthesis because generally require multistep synthesis, high energy-cost. Here, a facile ambient temperature synthesis of trimetallic NiCoFe-MOF nanostructures was reported, and then heat treated in nitrogen atmosphere to prepare NiCo/Fe3O4-MOF, which exhibit abundant active sites without destroy the nanostructure. Bisphenol A (BPA) is the most studied compound among the bisphenol group. Many countries have banned the use of BPA because of its toxic effect, which cause many adverse health effects in humans. Therefore, it is important to develop fast identification methods for the removing of BPA in the environment. The material had good removal efficiency on BPA in water environment with the removal efficiency of 88 ± 1.9% within 2 min, and the maximum adsorption capacity reached 53.92 ± 1.27 mg/g.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.3,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146258293","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":"Improved Method for PFAS in Environmental Waters.","authors":"Amanda N Belunis, William R LaCourse","doi":"10.1093/chromsci/bmag007","DOIUrl":"https://doi.org/10.1093/chromsci/bmag007","url":null,"abstract":"<p><p>Per- and polyfluoroalkyl substances (PFAS) are an emerging group of environmental contaminants widely used in consumer products. Public unease regarding the levels of these compounds in the environment has called for methods to keep up with emerging PFAS and regulations. There is a need for analytical methods that are efficient and robust that can be readily used and easily accessed in commercial laboratories. This work discusses the development of an efficient, sensitive and reliable liquid chromatography tandem mass spectrometry method for the analysis of 40 PFAS in aqueous matrices (10 min run time). Initial calibration demonstrated excellent linearity for all PFAS analytes with r 2 values greater than 0.997. Limit of detections (0.2-100 ng/L) and limit of quantifications (1-350 ng/L) show the ability for the method to reach necessary levels to stay up to date with federal and state regulations. Two solid phase extraction techniques were compared based on recovery accuracy and precision. Recoveries ranged from 92.0% to 105.0% and 67.0% to 109.0% for the automated and manual setups, respectively. Evidence was found to support improvements in sample recovery using an automated setup. The validated method was used to analyze samples from six natural water sources in the Baltimore-Metro area, where seven of the forty PFAS compounds were found in at least one sample.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.3,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147468163","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}
Rinkal Patel, Kunjal L Vegad, Shailvi B Joshi, Sarita J Gagat, Nikunj D Patel
{"title":"Non-targeted HPTLC Fingerprint Profiling for Swift Authentication of trikatu churna Coupled with Chemometric Methods.","authors":"Rinkal Patel, Kunjal L Vegad, Shailvi B Joshi, Sarita J Gagat, Nikunj D Patel","doi":"10.1093/chromsci/bmag008","DOIUrl":"10.1093/chromsci/bmag008","url":null,"abstract":"<p><p>\"Trikatu churna,\" very famous herbal formulation which is widely used and prescribed for various disease conditions like hypothyroidism, hyperlipidaemia, atherosclerosis and others. It is having well proven anti-inflammatory, hepatoprotective and anthelmintic activities. The preliminary issues in quality of trikatu churna arise due to numerous factors like replacement, omission and adulteration in key ingredients of trikatu churna with spurious alike ingredients. A novel, simple, swift, precise, robust, non-destructive and non-targeted method based on High Performance Thin layer chromatography (HPTLC) coupled with multicomponent analysis was developed to appraise the quality of the samples of trikatu churna. Ten market samples and one standardized in-house sample was used for quality evaluation. Three in house samples were also prepared by deliberately omitting one key ingredient in each. Various chemometrics methods like Principal Component Analysis, and Cluster Analysis based on Hierarchy for further analysis to evaluate the differences in market samples of trikatu churna. Thus, developed method can be used as an effectual and applied approach for quality assessment of trikatu churna.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147468081","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}
Yuan Chen, Tolulope Adebusuyi, Edwina Oppong, Edidiong Abraham, Yen Maroney Lawrence, Jing Ma, Dong Liang, San L Pham, Frank E McDonald, Alira Danaher, Daqing Wu, Huan Xie
{"title":"Method Development and Validation of Liquid Chromatography Tandem Mass Spectrometry for SLP-1A6 in Rat Plasma.","authors":"Yuan Chen, Tolulope Adebusuyi, Edwina Oppong, Edidiong Abraham, Yen Maroney Lawrence, Jing Ma, Dong Liang, San L Pham, Frank E McDonald, Alira Danaher, Daqing Wu, Huan Xie","doi":"10.1093/chromsci/bmag004","DOIUrl":"10.1093/chromsci/bmag004","url":null,"abstract":"<p><p>SLP-1A6 is a nicardipine-derived analog that modulates the embryonic ectoderm development/Enhancer of Zeste Homolog 2 axis and holds promise as novel therapeutics for castration-resistant prostate cancer (PCa). We report here the development and validation of a robust, sensitive and specific LC-MS/MS method for quantifying SLP-1A6 in rat plasma, as part of its preclinical investigation. The method demonstrated excellent linearity, precision, accuracy, extraction recovery and stability with negligent matrix effect over a 5-2500 ng/mL concentration range. The method was successfully applied for a single intravenous dose pharmacokinetic (PK) study in adult male Sprague-Dawley rats and the resulting PK parameters were comparable to those of nicardipine, indicating that SLP-1A6 retains the favorable PK profile of the parent compound while offering in vivo efficacy for chemoresistant PCa. These findings support the further preclinical development of SLP-1A6 to overcome chemoresistance in PCa.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13089522/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146194819","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":"Analysis of Tasimelteon in Pharmaceutical Formulations and Bulk Based on Design-Based Quality Approach by HPLC and Greenness Evaluation of the Method.","authors":"Saniye Özcan, Elif Özge Erkan","doi":"10.1093/chromsci/bmag005","DOIUrl":"10.1093/chromsci/bmag005","url":null,"abstract":"<p><p>In this study, a straightforward, precise, environmentally friendly, and strong high-performance liquid chromatography technique was established for the examination of Tasimelteon in pharmaceutical formulations. The chemometric factor screening investigation facilitated the identification of crucial technique parameters, which were subsequently improved using the Box-Behnken design to enhance comprehension and enhance the performance of the method. The separation was achieved with using the Supelco Ascentis® Express C8 column (100 × 4.6 mm, id, 2.7 μm) with a mobile phase consisting of methanol:phosphate buffer (0.030 M, pH 2.5) at a ratio of 51:49 (v/v). The flow rate was chosen as 1.2 mL/min. The optimized method was fully validated according to International Council on Harmonization (Q2)R1. The method demonstrated linearity within the concentration range of 10.0 to 75.0 μg/mL, with a coefficient of determination (R2) of 0.999 and a significance level (P) of less than 0.05. Linearity investigations were conducted using the peak normalization approach. The internal standard that was deemed most suitable was agomelatine, at a concentration of 33.0 μg/mL. In addition, the environmental sustainability of the method was proved using different analytical greenness metrics as National Environmental Methods Index, analytical eco-scale, Analytical Greenness Metric and Green Analytical Procedure Index for evaluating its greenness. The applicability of the method was demonstrated in the analysis of Hetlioz® pseudo formulation.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147463279","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}
Shaohua Zheng, Lina Zhang, Guanjun Nan, Guangde Yang, Bowen Shi
{"title":"Development and Validation of an HPLC Method for Determination of the Accumulation Patterns of Coumarin and 2-Hydroxycinnamic Acid in Different Parts of Eupatorium Fortunei Turcz. During Growth Stages.","authors":"Shaohua Zheng, Lina Zhang, Guanjun Nan, Guangde Yang, Bowen Shi","doi":"10.1093/chromsci/bmag001","DOIUrl":"10.1093/chromsci/bmag001","url":null,"abstract":"<p><p>To quantify coumarin and 2-hydroxycinnamic acid in Eupatorium fortune Turcz. (EFT), a high-performance liquid chromatography method was developed and rigorously validated. This optimized approach was subsequently applied to analyze the distribution patterns of both compounds across different plant tissues and at various growth stages. The results indicated that the contents of coumarin and 2-hydroxycinnamic acid varied significantly among plant parts and over time. Specifically, the concentrations in leaves substantially exceeded those in stems and roots, establishing the following concentration gradient: leaves > stems > roots. Throughout the growth cycle, the levels of both compounds exhibited two distinct peaks amid a general declining trend. Based on these accumulation dynamics, two harvest periods are recommended within one growth cycle: the optimal harvest time occurs in early May, with a secondary period in early July. Furthermore, the leaves were identified as the most promising medicinal tissue due to their markedly higher bioactive content. These findings offer valuable insights for improving the quality control and agricultural practices related to EFT.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146194739","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}