Chromatographia最新文献

{"title":"Analyzing the Volatile Flavor Components in Shanyao Yogurts","authors":"Yu Zhang,&nbsp;Fuli Li,&nbsp;Jiahui Liu,&nbsp;Jingchun Wang,&nbsp;Chaozheng Zhang","doi":"10.1007/s10337-025-04408-5","DOIUrl":"10.1007/s10337-025-04408-5","url":null,"abstract":"<div><p>To comprehensively investigate the flavor characteristics of Shanyao yogurt, headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC–MS) and headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) techniques were employed to analyze volatile flavor compounds(VFCs) in Shanyao yogurts fermented with <i>Lactobacillus rhamnosus</i> and <i>Lactobacillus plantarum</i>. The findings of the two techniques revealed variations in both components and concentrations of VFCs in the same sample. HS-SPME-GC-MS exhibited excellent performance in detecting acidic substances, while HS-GC-IMS demonstrated advantages in analyzing ester substances. Only 4 compounds were identified by both methods in Shanyao yogurt fermented by <i>L. plantarum</i>; whereas 7 compounds were identified by both methods in Shanyao yogurt fermented by <i>L. rhamnosus</i>. This research underscored the benefits of employing diverse analytical techniques for studying yogurt samples, as integrating multiple approaches provided a more comprehensive understanding of VFCs in Shanyao yogurt, thereby offering robust support for investigating VFCs in similar products.</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 5","pages":"423 - 432"},"PeriodicalIF":1.3,"publicationDate":"2025-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145163551","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 Role of Artificial Intelligence and Machine Learning in Polymer Characterization: Emerging Trends and Perspectives","authors":"Rick S. van den Hurk,&nbsp;Bob W. J. Pirok,&nbsp;Tijmen S. Bos","doi":"10.1007/s10337-025-04406-7","DOIUrl":"10.1007/s10337-025-04406-7","url":null,"abstract":"<div><p>The application of artificial intelligence (AI) and machine learning (ML) is rapidly expanding and has begun to make a significant impact on polymer development and characterization. This perspective article explores the current state of AI in this field and highlights areas where its potential remains underutilized. While the optimization of polymer synthesis to achieve desired properties and the classification of polymer types are well-established, opportunities for AI integration in detailed characterization, analytical method development, and data processing remain largely untapped. Greater automation of the analytical laboratory, whether through dedicated algorithms or AI-driven solutions, will enable analytical chemists to focus more on addressing research questions and interpreting results, rather than on method development and routine measurements.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 5","pages":"357 - 363"},"PeriodicalIF":1.3,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12116698/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144179761","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and Validation of QBD-Assisted Using Central Composite Design RP-HPLC Method for Lobeglitazone Sulfate and Glimipiride in Bulk and Its Combined Dosage Form","authors":"A. Marina Juliet,&nbsp;Punniyakoti Veeraveedu Thanikachalam","doi":"10.1007/s10337-025-04404-9","DOIUrl":"10.1007/s10337-025-04404-9","url":null,"abstract":"<div><p>The simultaneous quantification bulk active pharmaceutical components and combined dosage forms is vital for ensuring quality control and therapeutic efficacy. This study addresses the need for a reliable analytical method for the simultaneous quantification of lobeglitazone sulphate (LBZ) and glimepiride (GPR), two drugs often used in the administration of type 2 diabetes. A review of existing literature reveals the absence of a quality by design (QbD)-assisted reverse phase high-performance liquid chromatography (RP-HPLC) method for this specific combination. Using a QbD approach, a robust RP-HPLC method was developed and optimized employing a central composite design (CCD). The Agilent Infinity 1270 Series HPLC system, equipped with a Zorbax SB 618 column (5 μm, 46 × 150 mm), was used. Method parameters were fine-tuned to achieve optimal resolution (7.6), tailing (1.8), and retention times of 5.6 min for LBZ and 8.6 min for GPR. The optimized mobile phase consisted of ACN:KH₂PO₄ buffer (pH 3.5, 50:50 v/v), a flow rate of 1 mL/min, and a detection wavelength of 227 nm. The developed method was validated as per current regulatory guidelines, demonstrating precision, accuracy, and sensitivity. These results underscore the effectiveness of a QbD framework in method development, ensuring reproducibility and robustness. This study highlights the broader potential of QbD-assisted analytical techniques in pharmaceutical research, paving the way for more efficient drug quality assessments and improved therapeutic outcomes across diverse drug combinations.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 5","pages":"381 - 393"},"PeriodicalIF":1.3,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161608","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":"Analytical Method Development Strategy for Controlling Two New Nitrosamine Drug Substance Related Impurities (NDSRIs) in a Pharmaceutical Drug Product for Treatment of a Rare Disease","authors":"Partha Mukherjee,&nbsp;Xin Yao,&nbsp;Nastry Brignol,&nbsp;Madison Chao,&nbsp;Steven Tuske,&nbsp;M. Osman Sheikh,&nbsp;Jon Brudvig,&nbsp;Sheela Sitaraman,&nbsp;Jill M. Weimer,&nbsp;Saroj Ramdas","doi":"10.1007/s10337-025-04405-8","DOIUrl":"10.1007/s10337-025-04405-8","url":null,"abstract":"<div><p>N-Nitrosamines are raised as having health consequences by the European Medical Agencies ICH M7(R2) guidance on <i>Assessment and control of DNA reactive (mutagenic) impurities in pharmaceuticals to limit potential carcinogenic risk</i>. It has been suggested that nitrosamines have carcinogenic potential, and efforts should be made to control them at acceptable and safe levels in drug substances (DS). The detection of nitrosamine drug substance related impurities (NDSRIs) historically has encountered considerable challenges in establishing compound specific acceptable intake (AI) limits. Often, a default low AI limit of 18 ng/day was assigned to the NDSRIs due to the lack of their toxicology data, prior to the introduction of the current Carcinogenic Potency Categorization Approach (CPCA). Developing analytical methods to quantify NDSRIs posed a challenge due to an extremely low Quantitation Limit (QL), not exceeding 10% of the AI limit based on a conservative Threshold of Toxicological Concern (TTC) approach. This work presents the method development strategy for two complex diastereomeric NDSRIs in miglustat, a recently commercialized rare disease drug. A predictive chemistry for NDSRI formation and organic synthesis earlier was followed by in silico assessments of potential mutagenicity and carcinogenicity. This paper describes the development of a highly sensitive analytical method with a QL of 6.9 ppb for the combined NDSRIs, in alignment with the regulatory recommendation at the time of this work. The validated method was employed for confirmatory testing of miglustat batches for the combined NDSRIs. The results were below QL, and no routine NDSRI testing was required for future drug product (DP) batch release. This novel approach may offer valuable insights into the numerous molecules in development that will now require rigorous nitrosamine assessment.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 5","pages":"395 - 409"},"PeriodicalIF":1.3,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168477","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 Simple Precipitation Method Combined with LC–MS/MS for the Simultaneous Determination of 14 Water-Soluble Vitamins and Metabolites in Human Serum","authors":"Qiaoling Jiang,&nbsp;Qiaoli Wu,&nbsp;Shuhang Chen,&nbsp;Tianfu Zeng,&nbsp;Xiaoyi Tong","doi":"10.1007/s10337-025-04401-y","DOIUrl":"10.1007/s10337-025-04401-y","url":null,"abstract":"<div><p>This study introduces a rapid LC–MS/MS method designed to simultaneously quantify 14 water-soluble vitamins and their metabolites in human serum. The protein precipitation with metaphosphoric acid and stable isotope dilution techniques are utilized in this method. An Agilent XDB C18 column and dynamic ionization mode switching are adopted, enabling the completion of a single sample analysis within 5 min. The method has undergone rigorous validation. The lower limits of quantification (LLOQs) range from 0.3 to 400 ng/mL, with recovery rates between 80 and 120%. Intra-day and inter-day relative standard deviations (RSDs) are below 15%. The matrix effects are controlled within ± 15%, and the analyte carryover is less than 20% of the LLOQ. The stability tests have demonstrated that samples remain stable at room temperature (25 °C) for 10 h, at − 20 °C for 7 days, and can withstand one freeze–thaw cycle. Extracted samples are stable in the autosampler (4 °C) for 24 h. The method was applied to serum samples from 150 healthy individuals. Non-parametric statistical analysis was carried out to establish clinical reference intervals, which provides valuable data for the clinical evaluation of vitamin and metabolite levels in serum.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 5","pages":"365 - 380"},"PeriodicalIF":1.3,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168476","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":"Preparation and Performance Evaluation of a Novel Epitope-Imprinted Polymer with Specific Recognition of Tumor Marker Matrix Metalloproteinase-9","authors":"Mei Tian,&nbsp;Xue Dong,&nbsp;Jie Zhang,&nbsp;Jun Zhang,&nbsp;Wenxin Liu,&nbsp;Yu Cheng,&nbsp;Suhong Wang,&nbsp;Zehui Wei","doi":"10.1007/s10337-025-04403-w","DOIUrl":"10.1007/s10337-025-04403-w","url":null,"abstract":"<div><p>A novel epitope-imprinted polymer with specific recognition of trace tumor marker matrix metalloproteinase-9 (MMP-9) was synthesized and successfully applied for the enrichment, separation, and detection of the human serum samples. Based on catalytic domain characteristics containing zinc ion binding sites of MMP-9, an MMP-9 C-terminal nonapeptide was selected as the antigenic determinant template, while zinc acrylate and choline chloride-methacrylic acid were chosen as functional monomers. After optimizing the preparation conditions through single factor and mixed orthogonal experiments, molecularly imprinted polymers (MIPs) with a maximum adsorption capacity of 3.59 mg/g and an imprinting factor of 2.50 were obtained. MIPs showed good repeatability and reproducibility, and better selectivity for similar proteins than NIPs, with a 99.97% adsorption rate for 5 µg/mL MMP-9, which coincided with the results from sodium dodecyl sulfate polyacrylamide gel electrophoresis. The recovery of human serum samples spiked with nonapeptide was 90.04%, with a relative standard deviation (RSD) of 2.3% (<i>n</i> = 5), and the recovery of human serum samples spiked with MMP-9 protein was 75.05%, with an RSD of 0.88% (<i>n</i> = 5). The developed method had a linear range of 1–10 ng/mL for MMP-9, with a detection limit of 0.41 ng/mL. The synthesized MIPs were convenient, cost-effective and consistent. The results showed that they had the potential to be used as novel adsorption and enrichment materials. Moreover, they could offer valuable references for the further preparation of highly specific MMP-9 adsorbents.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 4","pages":"331 - 343"},"PeriodicalIF":1.2,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786437","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":"Congress, Conferences, and Workshops","authors":"","doi":"10.1007/s10337-025-04402-x","DOIUrl":"10.1007/s10337-025-04402-x","url":null,"abstract":"","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 4","pages":"355 - 356"},"PeriodicalIF":1.2,"publicationDate":"2025-03-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786672","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":"Green High-Performance Thin-Layer Chromatography: A Step Towards Eco-Friendly Analysis","authors":"Swecha Singh,&nbsp;Nazish khan,&nbsp;Tanushree Sawant,&nbsp;Radhika Raheja","doi":"10.1007/s10337-025-04397-5","DOIUrl":"10.1007/s10337-025-04397-5","url":null,"abstract":"<div><p>High-performance thin-layer chromatography (HPTLC) is a simple but reliable, sensitive, economical, and environmentally benign analytical technique for pharmaceuticals and herbal samples. Its advantages towards quantitative analysis include accurate sample application, quicker and efficient resolution of mixtures, minimum solvent usage and reduced sample size. The ability of HPTLC to examine numerous samples of varying complexity simultaneously and in parallel sets it apart from HPLC. This allows for a high sample throughput and the consumption of solvent and energy is low per sample. Furthermore, compared to HPLC, the use of HPTLC can conserve environmental resources because it requires little to no sample pre-treatments such as liquid–liquid extraction or solid-phase extraction. Several research studies on analytical method development using HPTLC now focus on the use of green solvents in lieu of traditional organic solvents, with the aim to reduce environmental pollution without compromising on analytical performance. In addition, advancements in assessment tools for determining “greenness”, such as AGREE (Analytical GREEnness metric approach and software), GAPI, NEMI, facilitate the evaluation of greenness for specific analysis. The green methods continue to offer rapid, sensitive, and environmentally friendly methodologies, complying with international guidelines of analytical techniques. Overall, the integration of green solvent-based HPTLC methods into analytical workflows represents a significant step towards sustainable and environmentally conscious analytical 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 4","pages":"287 - 302"},"PeriodicalIF":1.2,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786647","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":"Ultrasonic Assisted Salting-Out Micro-Liquid–Liquid Extraction Followed by Gas Chromatography for Determination of Ethanolamines in Sweetening Natural Gas Solutions","authors":"Sajjad Beheshti,&nbsp;Mehdi Vahidi,&nbsp;Maryam Abbasghorbani,&nbsp;Bahman Farajmand","doi":"10.1007/s10337-025-04399-3","DOIUrl":"10.1007/s10337-025-04399-3","url":null,"abstract":"<div><p>The high solubility of ethanolamines in the aqueous solutions is a big challenge for extracting these compounds. To overcome this problem, in this research, an easy sample preparation method based on salting-out micro-liquid–liquid extraction has been introduced to extract ethanolamines from aqueous samples, and determination has been done by gas chromatography-flame ionization detector (GC-FID). The solvent 1-propanol demonstrated significantly greater extraction efficiency than other solvents, including tetrahydrofuran, acetonitrile, and diethyl carbonate. Different variables affecting the extraction and derivatization of the target compounds were also investigated and optimized. The highest response was achieved with NaCl at a concentration of 35%, using 1000 µL of 1-propanol, a sonication power of 30 W for 20 s, a derivatization agent volume of 25 µL, and a derivatization time of 5 min. The analytical performances of the method were evaluated in optimal conditions. The linear ranges varied from 2 to 4000 mg/L, depending on the compound. The method demonstrated good repeatability, with relative standard deviations ranging from 2.4 to 10.3%. Limit of detections (LODs) were in the range of 0.5–2.3 mg/L. The method was finally used to determine ethanolamines in the commercial sweetening solutions. The relative recoveries (RR%) were achieved between 89 and 111%.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 4","pages":"303 - 310"},"PeriodicalIF":1.2,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786449","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":"Measurement of Diketene Using In Situ Derivatization-Headspace-Gas Chromatography","authors":"Noémi Göröcs,&nbsp;Balázs Volk","doi":"10.1007/s10337-025-04398-4","DOIUrl":"10.1007/s10337-025-04398-4","url":null,"abstract":"<div><p>During the registration procedure of a drug substance, the actual and potential impurities must be summarized in a legal documentation. Diketene is a reactive chemical compound which is used for the introduction of an acetoacetyl structural unit into organic compounds. Since this material commonly used as a reagent in the pharmaceutical industry, it is a potential impurity of certain drug substances. The aim of this work was to develop and validate a suitable method for the analysis of diketene by means of decomposition headspace gas chromatography. The product of the derivatization reaction is acetone, which can be easily measured by gas chromatography. Various parameters have been integrated into the elaborated limit test validation, such as specificity, detection limit (LD), quantification limit (LQ), system precision, recovery at limit level, robustness and solution stability. The limits of detection and quantification are 60 and 200 ppm, respectively. Using the above-mentioned new analytical method, the concentration of diketene can be determined accurately. These precise measurements are necessary for the appropriate characterization of the drug substance, which is a prerequisite step of a marketing authorization for the finished product.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 4","pages":"279 - 285"},"PeriodicalIF":1.2,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786513","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}