Chromatographia最新文献

{"title":"N-Nitroso-Vildagliptin, A New N-Nitrosamine Drug Substance Related Impurity (NDSRI) of Vildagliptin- An Antidiabetic Drug: Synthesis, Characterization and Development of Sensitive LC–MS/MS Method","authors":"Vipin Kumar,&nbsp;Lingaiah Balthu,&nbsp;Sriram Pepakayala,&nbsp;Yogesh Kumar Lohia,&nbsp;Deepika Kathuria,&nbsp;Priyanka Mathur,&nbsp;Vikas Rathod,&nbsp;Swapnil Sonar,&nbsp;Sumit S. Chourasiya","doi":"10.1007/s10337-025-04437-0","DOIUrl":"10.1007/s10337-025-04437-0","url":null,"abstract":"<div><p>The <i>N</i>-nitroso-vildagliptin impurity has been classified as genotoxic. According to the EMA, this impurity must be controlled within a limit of 15 ppm in the vildagliptin drug substance. This work demonstrates the synthesis and characterization of the <i>N</i>-nitroso-vildagliptin impurity using IR, NMR, and LC–MS techniques. The synthesized <i>N</i>-nitroso-vildagliptin impurity was used as a reference standard for the development and validation of an LC–MS/MS method, achieving a limit of detection (LOD) of 0.44 ppm and a limit of quantification (LOQ) of 1.46 ppm.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"791 - 799"},"PeriodicalIF":1.3,"publicationDate":"2025-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223754","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":"Absolute Molar Mass Determination in Mixed Solvents. 3. Accuracy of ∂n/∂c Values Obtained by Assuming 100% SEC Mass Recovery","authors":"André M. Striegel","doi":"10.1007/s10337-025-04438-z","DOIUrl":"10.1007/s10337-025-04438-z","url":null,"abstract":"<div><p>Accurate values of the specific refractive index increment (∂<i>n</i>/∂<i>c</i>) are essential to the accurate determination of molar mass averages, distributions, and related macromolecular parameters by, among others, size-based separations with online static light scattering and differential refractive index (DRI) detection. Examined here is the 100% mass recovery method of calculating the ∂<i>n</i>/∂<i>c</i> of dilute macromolecular solutions, when employing mixed solvents in a size-based separation (e.g., size-exclusion chromatography or SEC) with DRI detection. This method has been used successfully in the past for determining the ∂<i>n</i>/∂<i>c</i> of various polyelectrolytes. It is quicker, generally simpler, and less sample-intensive than its offline, batch-mode DRI counterpart. Whether or not the 100% mass recovery method allows for the necessary solvent equilibration within the immediate vicinity of the polymer chain during a chromatographic run, so as to allow for accurate determination of ∂<i>n</i>/∂<i>c</i> in SEC/DRI experiments, is evaluated here. This is done using a set of three narrow-dispersity linear polystyrene standards covering a 40-fold range in molar mass, dissolved in a 25:75 mix of tetrahydrofuran and <i>N</i>,<i>N-</i>dimethyl formamide. Results are compared to those previously obtained by the batch-mode method and from calculations involving the accurately known molar masses of the polymers and refractive indices of the solvents. The 100% mass recovery method of obtaining ∂<i>n</i>/∂<i>c</i> values, while of great help for determining the ∂<i>n</i>/∂<i>c</i> of, e.g., polyelectrolytes, does not appear able to overcome the obstacle of preferential solvation when analyzing macromolecules in a mix of non-isorefractive solvents with dissimilar second virial coefficients.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"801 - 805"},"PeriodicalIF":1.3,"publicationDate":"2025-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-025-04438-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223757","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":"Evaluation of Phthalate Esters Presence in Medical Devices’ Materials in France","authors":"Sacha Pérocheau Arnaud,&nbsp;Christian Saadé Abou Jaoudé,&nbsp;Sandra Olivero,&nbsp;Patrick Navard,&nbsp;Alice Mija,&nbsp;Veronique Michelet,&nbsp;Veronique Mondain","doi":"10.1007/s10337-025-04412-9","DOIUrl":"10.1007/s10337-025-04412-9","url":null,"abstract":"<div><p>A simple and efficient strategy was developed for the identification of material devices’ polymers and the extraction of the additives contained within. In this study, the focus is put on the presence of phthalate esters in French medical devices, mainly on diethylhexyl phthalate (DEHP), being reported as toxic, endocrine disruptor plasticisers. Their presence was investigated across seven standard medical devices, especially concerning newborn exposure, and compared with results obtained in similar materials from the past decades. Only traces of DEHP, below the limit of quantification (&lt; 6 ppm) were detected in one of the samples by GC–MS using a standard for identification and quantification. This study shows that phthalates’ presence in medical devices used in French hospitals has been greatly diminished, to the benefit of healthier hospital environments.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"737 - 741"},"PeriodicalIF":1.3,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-025-04412-9.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223742","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":"Simultaneous Determination of 14 Aconitum Alkaloids in Blood and Urine by SLE-UPLC-MS/MS","authors":"Yan Zhang,&nbsp;Li Ling,&nbsp;Liangjiao Qu,&nbsp;Wenyan Huang,&nbsp;Hongyan Zou","doi":"10.1007/s10337-025-04436-1","DOIUrl":"10.1007/s10337-025-04436-1","url":null,"abstract":"<div><p>Aconitum alkaloid poisoning which can lead to malignant arrhythmia, cardiogenic shock and even death has been frequently reported due to improper intake of <i>Aconitum</i> species in hospital emergency rooms. In this study, a simple method for simultaneous determination of 14 aconitum alkaloids in human blood and urine by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) was developed. Blood and urine samples were purified by supported liquid extraction (SLE) and analyzed by UPLC-MS/MS. Good linear relationships for 14 <i>aconitum</i> alkaloids were obtained in the corresponding range of 0.1–50 ng mL⁻¹ with correlation coefficients greater than 0.999 and detection limits of between 0.002 and 0.019 ng mL⁻¹. The average recoveries measured at three concentration levels ranged from 80.0% to 110.1% and 85.0% to 110.2% in spiked blood samples and urine samples, respectively, with the relative deviation less than 10%. The blood matrix effects ranged from 88.3% to 109.8%, while the urine matrix effects ranged between 91.4% and 103.6%. Both the intra-day and inter-day precisions were less than 11%. Finally, the method was successfully applied to the determination of <i>aconitum</i> alkaloids in the blood and urine of clinic poisoned patients showing its good potential for poison diagnosis in clinical emergency cases.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"779 - 790"},"PeriodicalIF":1.3,"publicationDate":"2025-08-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223753","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":"Effects of Silane Chemical Structures on the Surface Properties of Silanized Cardboard: Inverse Gas Chromatography and Complementary Analysis","authors":"Joonyeong Kim","doi":"10.1007/s10337-025-04434-3","DOIUrl":"10.1007/s10337-025-04434-3","url":null,"abstract":"<div><p>In this study, silanized cardboard samples (HSi-CB, MeSi-CB, EtSi-CB, and PrSi-CB) were prepared by reacting bare cardboard with ethoxysilane/chlorosilanes bearing different substituents (H-, CH₃-, CH₃CH₂-, and CH₃CH₂CH₂-) in toluene. Characterization using FTIR spectroscopy, elemental analysis, and surface area/pore volume measurements confirmed successful silanization, with HSi-CB exhibiting the largest amount of grafted silanes and branched polymeric/oligomeric siloxane networks. However, inverse gas chromatography (IGC) revealed that MeSi-CB exhibited the highest adsorption affinity toward hydrocarbons due to its larger dispersive surface energy <span>(left( {mathop gamma nolimits_{{text{S}}}^{{text{D}}} } right))</span> , resulting from grafted methylsilane groups, reduced hydroxyl groups, and the formation of micropores and channels via siloxane condensation. In contrast, EtSi-CB and PrSi-CB displayed lower <span>(mathop gamma nolimits_{{text{S}}}^{{text{D}}})</span> values due to the grafting of fewer silane groups and the limited formation of branched siloxane networks. Although HSi-CB exhibited the highest amount of silanes, its <span>(gamma_{{text{s}}}^{{text{D}}})</span> values remained comparable to those of bare cardboard. These results underscore the critical role of surface dispersive components and micropore/channel formation in boosting the adsorption performance of silanized cardboard. These results also provide valuable insights for the development of more efficient adsorbents for hydrocarbon capture and separation applications.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"759 - 770"},"PeriodicalIF":1.3,"publicationDate":"2025-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223755","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 a High-Performance Liquid Chromatography Method for the Detection of Rose Bengal in Canine Plasma","authors":"Sherry Cox,&nbsp;Madeline Duncan,&nbsp;Riley Golias,&nbsp;Julia Cutchin,&nbsp;Nora Springer,&nbsp;Aaron Bloom,&nbsp;Joan Bergman","doi":"10.1007/s10337-025-04435-2","DOIUrl":"10.1007/s10337-025-04435-2","url":null,"abstract":"<div><p>A straightforward and precise technique for the analysis of Rose Bengal concentrations in canine plasma was established and validated using HPLC. Following a simple protein precipitation method with methanol, separation occurred on an XBridge Phenyl column with a mobile phase of 10 mM ammonium phosphate and acetonitrile (65:35, v/v). Rose Bengal and meloxicam, the internal standard, were confirmed by monitoring UV–visible wavelengths at 549 nm and 370 nm, respectively. The lower limit of quantification (LLOQ) was determined to be 25 ng mL⁻¹ in a 100 μL sample. The recovery was greater than 90% while intra-assay variability was less than 5%. Inter-assay variability was less than 7%. This method could be useful in pharmacokinetic studies.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"771 - 777"},"PeriodicalIF":1.3,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223756","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":"Quality-by-Design-Driven Stability-Indicating Reverse-Phase High-Performance Liquid Chromatographic Method for Puerarin Quantification in Marketed Formulation and Lipid–Polymer Nanoparticles","authors":"Shivaraj Hooli,&nbsp;Kishori P. Sutar,&nbsp;Sankalp S. Sammasagi,&nbsp;Mahendra Kumar Chouhan","doi":"10.1007/s10337-025-04427-2","DOIUrl":"10.1007/s10337-025-04427-2","url":null,"abstract":"<div><p>Parkinson’s disease is a progressive neurodegenerative disorder with an increasing global prevalence, necessitating advanced therapeutic and analytical approaches. Puerarin, a phytoconstituent from <i>Pueraria lobata</i> (Kudzu), has therapeutic potential in respiratory illnesses, neurological diseases, psoriasis, and viral infections. However, puerarin quantification remains challenging due to complex methods, prolonged retention times, and missing stability-indicating degradation studies in published data. This study develops a simple, reliable, rapid, and cost-effective reverse-phase high-performance liquid chromatography method for quantifying puerarin in marketed and nanoformulations. A central composite design enabled statistical optimization, fewer experimental runs, and critical analytical attributes. The method was validated as per ICH (Q2R1) guidelines. Chromatographic conditions included an acetic acid buffer (0.1%, pH 3.2):methanol (50:50, v/v) mobile phase, a 1 mL min⁻¹ flow rate and a 250 nm detection wavelength, achieving a puerarin retention time of 3.1 min. The linear calibration curve (<i>R</i>² &gt; 0.999) had LOD and LOQ values of 0.2148 µg mL⁻¹ and 0.6511 µg mL⁻¹, respectively. Precision studies (intra-day and inter-day) showed an RSD below 2% with consistent recovery. The method quantified puerarin in marketed and nanoformulations with 102.29% and 98.84% efficiency. Stress degradation studies confirmed robustness. The developed method provides a reasonably lower retention time and its validation produces quality data compared with publications resembling a problem-solving approach for quantifying puerarin. This validated method provides an accurate, precise, and economical strategy for puerarin quantification in pharmaceuticals.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 10","pages":"743 - 757"},"PeriodicalIF":1.3,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-025-04427-2.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145223743","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 Application of an Optimised HPTLC Method for Profiling Bioactive Compounds in Marketed Green Tea Products","authors":"Sanjib Kumar Panda,&nbsp;Nilima Mohanty,&nbsp;Pallavi Khuntia,&nbsp;Aakankhika Ray,&nbsp;Ashwini Mallad,&nbsp;Deepak Jena","doi":"10.1007/s10337-025-04431-6","DOIUrl":"10.1007/s10337-025-04431-6","url":null,"abstract":"<div><p>Green tea has gained the global recognition for its health-promoting bioactive components such as rutin, caffeic acid, chlorogenic acid, and caffeine. With increasing consumer demand and rising concerns over product authenticity and adulteration, this study presents a qualitative high-performance thin-layer chromatography (HPTLC) for profiling these four marker compounds in five commercially available green tea products compared against a botanical reference material (BRM). The HPTLC method was developed for identifying these compounds using a mobile phase mixture of ethyl acetate, methanol, water, and formic acid (50:4:4:2.5). Additionally, physiochemical differences of green tea samples were also studied, including colour, texture, pH, and solubility in water, providing further insights into product quality and authenticity. This approach contributes to the utility of qualitative HPTLC as a cost-effective, rapid screening tool for standardization and quality control of green tea formulations. The findings are precise and relevant, supporting regulatory and consumer safety to ensure the integrity of green tea supplements in a growing global market.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"727 - 735"},"PeriodicalIF":1.3,"publicationDate":"2025-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011944","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":"Optimizing Internal Standard Selection for Precise Bioanalytical Quantification of Antidiabetic Drugs: A Critical Review","authors":"Sanket Jadhav,&nbsp;Sandip Auti,&nbsp;Sanjay Sharma","doi":"10.1007/s10337-025-04432-5","DOIUrl":"10.1007/s10337-025-04432-5","url":null,"abstract":"<div><p>Accurate quantification of antidiabetic drugs within biological matrices is essential for pharmacokinetic, pharmacodynamic, and therapeutic monitoring. Internal standards (ISs) play a pivotal role in ensuring the precision, accuracy, and reproducibility of bioanalytical assays by compensating for matrix effects, instrumental fluctuations, and inconsistencies in sample preparation. This review systematically examined 73 research articles to discern trends in IS selection, extraction techniques, biological fluid distribution, and analytical methodologies employed for quantifying antidiabetic drugs. The study elucidates the rationale behind IS selection, including the utilization of stable isotope-labeled (SIL) compounds, structurally related drugs, and deuterated analogs, which enhance the reliability and robustness of the method. Furthermore, the review underscores the significance of optimizing sample preparation techniques, such as protein precipitation (PP), liquid–liquid extraction (LLE), and solid-phase extraction (SPE), to improve analyte recovery. Advanced chromatographic and mass spectrometric techniques, particularly LC–MS/MS and HPLC/UPLC–MS/MS, provide high sensitivity and specificity along with broad calibration ranges, facilitating precise drug concentration measurements. These findings highlight the necessity for standardized IS selection criteria and refined bioanalytical methodologies to ensure reliable quantification across diverse biological fluids. By addressing existing challenges and proposing best practices, this review contributes to the advancement of bioanalytical research in diabetes management, aiding the optimization of pharmacokinetic studies and therapeutic monitoring of diabetes. The insights presented herein are crucial for enhancing the accuracy of drug quantification, thereby facilitating improved clinical decision-making and the development of more effective antidiabetic therapies.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"637 - 657"},"PeriodicalIF":1.3,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011765","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":"Sustainable HPLC Method for Resmetirom, a Novel THR-β Agonist: Development, Validation and Greenness Assessment","authors":"Khushi Dahiya,&nbsp;Sanjay Sharma","doi":"10.1007/s10337-025-04429-0","DOIUrl":"10.1007/s10337-025-04429-0","url":null,"abstract":"<div><p>Resmetirom (RMT), a new drug approved for the treatment of metabolic dysfunction-associated steatohepatitis and the present work describes the development and validation of a reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of RMT. The technique utilizes a Kromasil C18 column with mobile phase Acetonitrile and Ammonium acetate buffer (pH 3.5) in a 70:30 ratio, flow rate 0.8 mL min⁻¹, and UV detection at 298 nm. The process was validated as per the ICH Q2 (R2) guidelines, exhibiting specificity, linearity (5–30 µg mL⁻¹, <i>R</i>² = 0.9951), precision (RSD &lt; 2%), accuracy (98–102% recovery), LOD of 0.214 µg mL⁻¹, and LOQ of 0.651 µg mL⁻¹. The method is applicable to the active pharmaceutical ingredient (API) and was successfully validated to estimate RMT content present in tablets prepared in-house. The proposed analytical method was evaluated for environmentally friendliness, assessed qualitatively and quantitatively using AGREE, cGAPI, AGREEPrep, and MoGAPI software. The validated RP-HPLC method gives a good and efficient means for quantifying RMT, is cost saving and time efficient thereby applicable in pharmaceutical quality control and analysis.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"717 - 725"},"PeriodicalIF":1.3,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011763","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}