Chromatographia最新文献

{"title":"Automated Extraction and Quantification of Immunosuppressants  and Anticonvulsants from Dried Blood Spots: Evaluation of Transcend DBSA–TLX-1–MS/MS System","authors":"Pragya Sharma,&nbsp;Alison Lightfoot,&nbsp;Richard G. Lahr,&nbsp;Chris Thompson,&nbsp;Jennifer Faber,&nbsp;Joshua Miller,&nbsp;Jingshu Guo,&nbsp;Loralie J. Langman,&nbsp;Paul J. Jannetto,&nbsp;Anthony Maus","doi":"10.1007/s10337-025-04421-8","DOIUrl":"10.1007/s10337-025-04421-8","url":null,"abstract":"<div><p>Immunosuppressants and anticonvulsant drugs are routinely quantified using liquid chromatography–tandem mass spectrometry (LC–MS/MS) in whole blood and serum, respectively, which necessitates frequent phlebotomy visits for patients. Alternatively, dried blood spots (DBS) measurements have the potential to reduce the cost of sample collection and shipping, while simultaneously enabling convenient at-home collection for patients. We evaluated Transcend™ DBSA–TLX-1–MS/MS System through method development and analytical validation for measurements of immunosuppressants (tacrolimus, sirolimus and everolimus) and anticonvulsants (levetiracetam and lamotrigine) in DBS. Given the relatively low analytical measurement interval (AMI) for these immunosuppressants, sufficient sensitivity is imperative, and the desired lower limit of quantitation (LLOQ) of 1 ng/mL was achieved, with an interday %CV less than 10% at the LLOQ. Conversely, the comparatively high AMI for the anticonvulsant drugs necessitated careful optimization to avoid saturation and minimize imprecision. For all analytes, carryover was minimal, and linearity and accuracy using spiked samples indicated adequate performance based on the regression comparisons. Therefore, our proof-of-concept study suggests that the DBSA–TLX-1–MS/MS has the potential to provide exceptional analytical performance, which will facilitate future clinical validations while minimizing labor required to perform DBS measurements.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"555 - 561"},"PeriodicalIF":1.3,"publicationDate":"2025-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037494","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":"The Origin of a ‘Ghost’ Peak in the Gas Chromatography of Certain Intact Amine Salts and the Potential Scope and Analytical Value of the Phenomenon Causing the Peak","authors":"Kenneth Paul Kirkbride,&nbsp;Paul Edwin Pigou","doi":"10.1007/s10337-025-04416-5","DOIUrl":"10.1007/s10337-025-04416-5","url":null,"abstract":"<div><p>When certain amine salts are subjected directly to gas chromatography (i.e., without prior derivatization or deprotonation) even when highly pure two or more peaks are observed, only one of which is due to elution of the amine freebase. These unexpected results are confusing to analysts and if inexplicable results such as these are presented as evidence in a court of law they erode confidence in forensic analysis. There is little discussion in the literature regarding the origins of one of the unexpected ‘ghost’ peaks. This article indicates that the particular ‘ghost’ peak under discussion is not a ghost at all, but a peak due to the analyte itself—it arises as a result of elution of intact amine salt or carry-over of a salt from a previous injection. Elution of HI or HBr amine salts using gas chromatography—mass spectrometry can readily be confirmed by searching for the presence of halide⁺ and hydrohalide⁺ ions, but confirmation of HCl salts requires the mass spectrometer’s scan range to commence at low m/z in order to avert analytical confusion. Certain amine salts, such as drugs and explosives, are very important in forensic chemistry and the development of methodology based upon gas chromatography for the analysis of these compounds in their intact salt forms (i.e., where the cation and anion pairing information is not lost) would be a valuable contribution to the field. Other fields of analytical chemistry, such as environmental monitoring and analysis of food and industrial products may also benefit from the development of a GC method for the analysis of intact amine salts. The results presented here suggest that further development of gas chromatography for the analysis of intact amine salts is warranted.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"521 - 529"},"PeriodicalIF":1.3,"publicationDate":"2025-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168255","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":"Determination of Major Anions in Human Serum by Capillary Zone Electrophoresis","authors":"Evgeniya V. Polyakova,&nbsp;Kirill N. Narozhnykh,&nbsp;Sofiya E. Romanova,&nbsp;Tatyana V. Skiba","doi":"10.1007/s10337-025-04415-6","DOIUrl":"10.1007/s10337-025-04415-6","url":null,"abstract":"<div><p>This study presents an optimized method for determining major anions (chloride, sulfate, phosphate, citrate, and lactate) in human serum using capillary zone electrophoresis (CZE) with indirect photometric detection. A comparative analysis was conducted to evaluate the effectiveness of an electroosmotic flow (EOF) modifier (cetyltrimethylammonium hydroxide—CTAOH) and an ion-pairing reagent (tetrabutylammonium hydroxide—TBAOH). The optimal electrolyte composition (10 mM chromate, 16 mM DEA, 0.5 mM CTAOH) was determined, ensuring high separation quality and detection sensitivity. An improved sample preparation method, involving protein precipitation with acetonitrile, was implemented. Achieved limits of detection were 6 mg/L for sulfate, 12 mg/L for phosphate, 10 mg/L for citrate, and 16 mg/L for lactate. The method’s validation characteristics (spike-recovery of 90–111%, relative standard deviation (RSD) ≤ 10%) demonstrate high accuracy and reproducibility.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"513 - 520"},"PeriodicalIF":1.3,"publicationDate":"2025-06-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168360","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":"Determination of Omeprazole and its Related Impurities in Bulk Drug Substance Batches by A Stability Indicating HPLC Method Based on a Short Octyl Fused Core Column","authors":"Renuka Rathnasekara,&nbsp;Daoli Zhao,&nbsp;Abu M. Rustum","doi":"10.1007/s10337-025-04418-3","DOIUrl":"10.1007/s10337-025-04418-3","url":null,"abstract":"<div><p>Omeprazole (OMP), a member of proton pump inhibitors class, is widely used in the treatment of dyspepsia and peptic ulcer disease, etc. A simple, robust, and stability-indicating reverse phase high performance liquid chromatography (RP-HPLC) method has been developed and validated for determination of OMP and its related substances. The analytes were separated on a short, fused core Halo octyl (C8) column (50 mm × 2.1 mm i.d., 2.7 µm particle size) using a gradient elution at a column temperature of 25 °C. Omeprazole and its related substances were monitored by UV detection at 280 nm. Mobile phase A (MPA) of the method is 10 mM ammonium acetate (NH₄OAc) in H₂O and mobile phase B (MPB) is MeOH/IPA (95/5). The total run time of the new method is 33 min. The new HPLC method has a significantly higher degree of selectivity and efficiency in separating OMP related compounds compared with the current compendial HPLC methods for OMP drug substance outlined in the United States and European Pharmacopeia monographs.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"501 - 512"},"PeriodicalIF":1.3,"publicationDate":"2025-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145167872","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 Quality-Driven, Eco-friendly High-Performance Thin-Layer Chromatography Method for Fluvoxamine Maleate Analysis in Tablets and MS Identification of its Degradation Products","authors":"Vidhya K. Bhusari,&nbsp;Prasad S. Giri,&nbsp;Minal R. Ghante","doi":"10.1007/s10337-025-04417-4","DOIUrl":"10.1007/s10337-025-04417-4","url":null,"abstract":"<div><h3>Introduction</h3><p>A common selective serotonin reuptake inhibitor used to treat depression and obsessive–compulsive disorder is fluvoxamine maleate. </p><h3>Objective</h3><p>The goal of this study was to develop and validate a HPTLC method for the analysis of fluvoxamine maleate in pharmaceutical dosage forms, utilizing a risk-based quality by design approach.</p><h3>Methods</h3><p>HPTLC method was optimized with a mobile phase composed of toluene: ethyl acetate: methanol: triethylamine in a ratio of 1: 5: 4: 0.1 (v/v/v/v). UV detection was performed at 257 nm. Studies on forced degradation were carried out in a variety of stress environments, including as thermal, oxidative, hydrolytic, alkaline, acidic, and photolytic conditions, to assess stability of fluvoxamine maleate. The degradation products were characterized using high-resolution mass spectrometry to identify potential impurities and degradation pathways.</p><h3>Results</h3><p>The developed method demonstrated excellent linearity over a concentration range of 100 to 600 ng/band, with a correlation coefficient of 0.9994 and the LOD and LOQ values were found to be 15.36 ng/band and 46.55 ng/band. The method was validated in accordance with ICH Q2(R1) guidelines, confirming its specificity, linearity, precision, accuracy, and robustness. The green chemistry aspects of the method were evaluated using Analytical Greenness Metric Approach and Software and Green Analytical Procedure Index, which highlighted the method’s eco-friendly characteristics. Additionally, the Blue Applicability Grade Index tool was used to assess the method’s practicality and suitability for routine pharmaceutical analysis, confirming its application in real-world settings.</p><h3>Conclusion</h3><p>The validated HPTLC method for analyzing fluvoxamine maleate in tablet dosage forms was robust, reliable, and accurate. It effectively identified and characterized degradation products, ensuring the consistent quality and safety of pharmaceutical products. The method offers a sustainable and efficient alternative for quality control in the pharmaceutical industry, combining rigorous validation with environmentally conscious practices.</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 6-7","pages":"483 - 499"},"PeriodicalIF":1.3,"publicationDate":"2025-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145167173","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":"Affinity Fishing of ACE Ligands from C. axillaris using Surface Functionalized Magnetic Nanoparticles","authors":"Xianhong Zhu,&nbsp;Min Zhang,&nbsp;Kunming Qin,&nbsp;Xueying Qin,&nbsp;Miaomiao Chi,&nbsp;Yan Zhang,&nbsp;Hongsen Wang,&nbsp;Xichen Song,&nbsp;Xun Gao","doi":"10.1007/s10337-025-04414-7","DOIUrl":"10.1007/s10337-025-04414-7","url":null,"abstract":"<div><p><i>Choerospondias axillaris (C. axillaris)</i>, recognized as an effective herbal remedy for coronary heart disease (CHD), has been clinically utilized. Although the angiotensin-converting enzyme (ACE) has been extensively investigated as a pertinent target for CHD treatment, there is currently limited research on screening potential ACE inhibitors from <i>C. axillaris</i>. To advance the broader utilization of <i>C. axillaris</i> in coronary heart disease treatment, the target active components of ACE in <i>C. axillaris</i> were analyzed through the integration of magnetic-targeted fishing technology with functionalized magnetic nanospheres. Magnetic nanospheres functionalized with GO@Fe₃O₄@SiO₂-ACE (SMGO-ACE) were characterized using a vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), and transmission electron microscope (TEM). The specific binding of lisinopril with the angiotensin-converting enzyme was employed to optimize the performance of the synthesized material and the relevant conditions during targeted fishing. Subsequently, five active ingredients were identified as (2R,3S)-Dihydrodehydroconiferyl alcohol, isovanillin, quinic acid, chrysin, and isorhamnetin. This study provides a precedent for the targeted extraction and separation of active ingredients in complex mixtures.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"473 - 482"},"PeriodicalIF":1.3,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145166996","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":"Design and Numerical Analysis of a Single Inlet-Based Spiral Microfluidic Chip for Separation of Circulating Tumor Cells and Blood Plasma Using the Inertial Focusing Approach","authors":"Writtick Pakhira,&nbsp;R. Kumar,&nbsp;Khalid Mohd. Ibrahimi,&nbsp;Rituraj Bhattacharjee","doi":"10.1007/s10337-025-04411-w","DOIUrl":"10.1007/s10337-025-04411-w","url":null,"abstract":"<div><p>Circulating tumor cells (CTCs) and blood plasma both work as biomarkers for the initial detection and diagnosis of metastatic cancers. Nowadays, with the development of microscale devices, for the separation of CTCs and blood plasma from normal cells, one of the most effective techniques is inertial focusing using microfluidic chips. The present research work reported a single inlet and single loop-based microfluidic chip for simultaneous separation of PC3 (prostate cancer) CTCs and blood plasma from normal blood cells using the inertial focusing approach. Two different sized PC3 CTCs and different inlet flow velocities corresponding to different Reynolds numbers are explored to accomplish optimum separation performance of the chip. Three-dimensional numerical simulations were executed with COMSOL Multiphysics 5.4 software and finite element method analysis. It has been confirmed that 100 % separation purity and cell recovery were achieved for both 17 µm and 20 µm PC3 CTCs at the Reynolds number of 67 and 65.67, respectively. The microfluidic chip also achieved a maximum plasma recovery of 54.87 % with 100 % purity. </p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"453 - 471"},"PeriodicalIF":1.3,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168582","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":"Optimization of SEC-HPLC Method for the Quantitative Estimation of a Process-Related Residual Impurity, Dimethylaminopyridine (DMAP) in the Manufacturing of Pneumococcal Polysaccharide Conjugates Vaccine","authors":"Swapan Kumar Jana,&nbsp;Avinash V. Kapase,&nbsp;Shital S. Jain,&nbsp;Vikas M. Kalbhor,&nbsp;Rahul S. Chowdhury","doi":"10.1007/s10337-025-04409-4","DOIUrl":"10.1007/s10337-025-04409-4","url":null,"abstract":"<div><p>The conjugation technology is used for the manufacturing of polysaccharide conjugate vaccines against pathogenic organisms like <i>Streptococcus pneumoniae</i>, <i>Haemophilus influenzae</i> type b, etc. Conjugation using CDAP chemistry is widely utilized because of high yield and short reaction time. The cyano group of CDAP is attached to hydroxyl group of polysaccharides, resulting in activated polysaccharide with generation of process-related residual impurity, dimethyl aminopyridine (DMAP) which should be &lt; 1.5 µg/day as per regulatory guidelines. In the present study, we reported the SEC-HPLC coupled with UV detector for quantitative estimation of residual DMAP content in pneumococcal polysaccharide–protein conjugates. The method was validated as per the ICH guidelines using representative pneumococcal conjugate of serotype 1, 6B and 23F. The method specificity was confirmed using placebo buffers and the identity of DMAP was ensured using orthogonal GC–MS method. The method showed linearity between 0.1 and 15 µg/mL with linear regression of &gt; 0.99. Detection and quantitation limits of 0.03 µg/mL and 0.1 µg/mL were observed respectively. The overall % RSD of DMAP content was found to be between 0.94 and 1.91% suggesting precision of the method. Accuracy was performed by spiking known amount of DMAP at six different concentration levels and % recovery of 87 to 104% was noted. The validated SEC-HPLC–UV method was successfully applied for various stages of pneumococcal polysaccharide conjugate vaccines including crude, in-process and final purified samples. This has suggested that the SEC-HPLC–UV method can be used as routine process analytical tool to monitor residual DMAP.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"441 - 451"},"PeriodicalIF":1.3,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145167645","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":"Flowing Dynamic Light Scattering with Potential to Improve Accuracy for Asymmetric Flow Field-Flow Fractionation","authors":"Guiqiong Huang,&nbsp;Bingquan Xu","doi":"10.1007/s10337-025-04410-x","DOIUrl":"10.1007/s10337-025-04410-x","url":null,"abstract":"<div><p>Asymmetric flow field-flow fractionation (AF4) separates constituents based on particle size and is emerging as a powerful tool for obtaining high-resolution information on the size of nanoparticles in liquid media. However, the size measurement inaccuracy has been reported for traditional dynamic light scattering (DLS) detectors when coupled to AF4 systems for the reason of additional component caused by uniform translation motions. In this paper, we developed a flowing DLS for AF4 study based on our sinc model reported previously. We further investigated the reliability of the size measurement provided by sinc model. The experiments were performed with suspensions of mono-dispersed polystyrene microspheres with a nominal diameter of 201 nm, 400 nm, 596 nm, and 799 nm at a range of different detector flow rates. The results obtained demonstrate that sinc model not only can measure the particle size but also flow velocity accurately. We believe our model can provide particle size information by coupling AF4 to DLS more accurately and pave the way for the complex AF4 system study, such as the electrical asymmetric flow field-flow fractionation in the flowing dispersion.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 6-7","pages":"433 - 440"},"PeriodicalIF":1.3,"publicationDate":"2025-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168056","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":"Standardized HILIC-FLD N-Glycan Analysis for Assessing N-Glycosylation Heterogeneity and Glycosylation-Related Quality Attributes in Bevacizumab from Multiple Manufacturers","authors":"Doudou Lou,&nbsp;Yuan Zhu,&nbsp;Jingke Fan,&nbsp;Lin Fan,&nbsp;Qingfu Zhu,&nbsp;Yihong Lu,&nbsp;Shuqiang Zhao","doi":"10.1007/s10337-025-04407-6","DOIUrl":"10.1007/s10337-025-04407-6","url":null,"abstract":"<div><p>N-glycosylation heterogeneity has a significant impact on the clinical safety, efficacy, pharmacokinetics (PK), and pharmacodynamics of monoclonal antibody (mAb) drugs, thus becoming a critical quality attribute (CQA) of great concern. In the registration quality standards for bevacizumab produced by different manufacturers, either lacking supervision of N-glycosylation or the detection methods and criteria vary greatly among manufacturers, leading to compromised comparability of results. Besides, the existing quality control system pays insufficient attention to the correlation between glyco-relevant physicochemical properties and glycosylated modification. In this study, a standardized hydrophilic interaction liquid chromatography-fluorescence detection (HILIC-FLD) N-glycan profiling method was developed, which had been proven to be more time-saving and easier to operate and was used for the parallel analysis of N-glycan profiles in bevacizumab products provided by 8 different manufacturers. We also paid attention to the glycosylation-related CQAs including charge heterogeneity, isoelectric point, non-glycosylated heavy chain (NGHC) and aggregates. Results revealed obvious difference in N-glycosylation, NGHC and aggregates among manufacturers. Among all the mAbs, the abundance of major glycoforms showed similar order yet the percentage of the same glycoform varies greatly. In summary, the standardized method could offer a reliable, efficient and practical approach for the parallel analysis and comparison of glycosylation and related CQA heterogeneity among manufacturers, providing a reference for more effective quality control of mAb drugs.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 5","pages":"411 - 422"},"PeriodicalIF":1.3,"publicationDate":"2025-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145164516","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}