Chromatographia最新文献

Preparation and Performance Evaluation of a Novel Epitope-Imprinted Polymer with Specific Recognition of Tumor Marker Matrix Metalloproteinase-9

IF 1.2 4区化学

Chromatographia Pub Date : 2025-03-21 DOI: 10.1007/s10337-025-04403-w

Mei Tian, Xue Dong, Jie Zhang, Jun Zhang, Wenxin Liu, Yu Cheng, Suhong Wang, Zehui Wei

{"title":"Preparation and Performance Evaluation of a Novel Epitope-Imprinted Polymer with Specific Recognition of Tumor Marker Matrix Metalloproteinase-9","authors":"Mei Tian, Xue Dong, Jie Zhang, Jun Zhang, Wenxin Liu, Yu Cheng, Suhong Wang, 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}

引用次数: 0

Congress, Conferences, and Workshops

IF 1.2 4区化学

Chromatographia Pub Date : 2025-03-18 DOI: 10.1007/s10337-025-04402-x

引用次数: 0

Green High-Performance Thin-Layer Chromatography: A Step Towards Eco-Friendly Analysis

IF 1.2 4区化学

Chromatographia Pub Date : 2025-03-14 DOI: 10.1007/s10337-025-04397-5

Swecha Singh, Nazish khan, Tanushree Sawant, Radhika Raheja

{"title":"Green High-Performance Thin-Layer Chromatography: A Step Towards Eco-Friendly Analysis","authors":"Swecha Singh, Nazish khan, Tanushree Sawant, 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}

引用次数: 0

Ultrasonic Assisted Salting-Out Micro-Liquid–Liquid Extraction Followed by Gas Chromatography for Determination of Ethanolamines in Sweetening Natural Gas Solutions

IF 1.2 4区化学

Chromatographia Pub Date : 2025-03-10 DOI: 10.1007/s10337-025-04399-3

Sajjad Beheshti, Mehdi Vahidi, Maryam Abbasghorbani, Bahman Farajmand

{"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, Mehdi Vahidi, Maryam Abbasghorbani, 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}

引用次数: 0

Measurement of Diketene Using In Situ Derivatization-Headspace-Gas Chromatography

IF 1.2 4区化学

Chromatographia Pub Date : 2025-03-05 DOI: 10.1007/s10337-025-04398-4

Noémi Göröcs, Balázs Volk

{"title":"Measurement of Diketene Using In Situ Derivatization-Headspace-Gas Chromatography","authors":"Noémi Göröcs, 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}

引用次数: 0

A Comprehensive Stability-indicating Method for Teriflunomide: Impurity Profiling and Degradation Analysis in Tablet Formulations

IF 1.2 4区化学

Chromatographia Pub Date : 2025-03-05 DOI: 10.1007/s10337-025-04400-z

Hande Gayretli, Egesen Halici, Bahar Koksel Ozgen, Nagehan Sarracoglu, Asuman Aybey Doganay, Onur Pinarbasli

{"title":"A Comprehensive Stability-indicating Method for Teriflunomide: Impurity Profiling and Degradation Analysis in Tablet Formulations","authors":"Hande Gayretli, Egesen Halici, Bahar Koksel Ozgen, Nagehan Sarracoglu, Asuman Aybey Doganay, Onur Pinarbasli","doi":"10.1007/s10337-025-04400-z","DOIUrl":"10.1007/s10337-025-04400-z","url":null,"abstract":"<div><p>This study presents a stability-indicating method for teriflunomide, a drug administered to adults for the treatment of multiple sclerosis (MS) in its various forms, including clinically isolated syndrome, relapsing–remitting, and active secondary progressive disease. The method, which has been validated comprehensively for both impurities and the assay, plays a key role in determining teriflunomide in tablet formulations. It successfully separates two specified degradation impurities in line with the European Pharmacopeia (EP) standards. To assess the stability of teriflunomide, the method subjects it to stress conditions such as acid/base hydrolysis, oxidation, photodegradation, and thermal degradation. Using a C18 column at 30 ℃, with a mobile phase of pH 3.4 solutions and acetonitrile at 0.8 mL/min, and UV detection at 248 nm, the method ensures the resolution of degradation products from the primary teriflunomide peak. The teriflunomide peak remained pure under all stress conditions, confirming the specificity and stability-indicating nature of the method. The validation followed FDA and ICH guidelines, with results for linearity, accuracy, precision, specificity, robustness, limit of detection, limit of quantification, and system suitability all meeting established acceptance criteria.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 4","pages":"311 - 321"},"PeriodicalIF":1.2,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786512","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}

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Stability-Indicating RP-HPLC Method for the Quantification of Daprodusdat in Pharmaceutical Formulation

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-17 DOI: 10.1007/s10337-025-04396-6

Hümeyra Funda Vardar, Sıdıka Ertürk Toker

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Thank You to Our Reviewers in 2024

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-13 DOI: 10.1007/s10337-025-04394-8

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Integrating Quality by Design and Green Chemistry for Sustainable Drug Development: Acalabrutinib Stability Study

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-12 DOI: 10.1007/s10337-025-04391-x

Anuj N. Nahata, Himanshu Pawar, Mital Patel

{"title":"Integrating Quality by Design and Green Chemistry for Sustainable Drug Development: Acalabrutinib Stability Study","authors":"Anuj N. Nahata, Himanshu Pawar, Mital Patel","doi":"10.1007/s10337-025-04391-x","DOIUrl":"10.1007/s10337-025-04391-x","url":null,"abstract":"<div><p>Regulatory agencies prioritize the safety and efficacy of pharmaceuticals. In this context, our research aims to develop a simple, sensitive, and eco-friendly LCMS-compatible high-performance liquid chromatography stability indicating analytical method (SIAM) technique to identify impurities in Acalabrutinib (ACB) under various stress conditions. This method is designed in compliance with ICH QIA (R2) and Q3, incorporating Green Chemistry principles and Quality by Design (QbD). To optimize the method, an ideal split-plot design was used to evaluate critical method parameters (CMPs), followed by a central composite design (CCD) to refine the conditions. Statistical analysis revealed <i>p</i> values < 0.001 for the model and 0.05 for lack of fit, indicating the most suitable statistical model for the evaluated responses (peak resolutions R1–R4). The optimized method attributes include an ACN:ammonium acetate buffer (pH 5) ratio of 50:50 (v/v), a flow rate of 0.8 mL/min, and a column oven temperature of 35 °C, derived from CCD. An isocratic elution method using the Waters e2998 HPLC Kromasil 100-5-C18 (250 × 4.6 mm; 5 µm) analytical column enabled superior separation of components, with a run time of 35 min and a wavelength of 254 nm. Stress studies revealed that ACB is sensitive to hydrolysis and photolytic conditions, with ACN identified as the most suitable diluent. Method validation was conducted according to ICH Q2 guidelines, and showed a correlation coefficient (<i>r</i><sup>2</sup>) exceeding 0.992, with RSD values (<i>n</i> = 6) ranging from 0.76 to 1.93% across the LOQ-150% range. Specificity studies confirmed no interference between impurities and active analytes. Through stress testing, 28 degradation products were identified, and the method was assessed for eco-friendliness using seven different tools, confirming its sustainable nature for pharmaceutical applications.</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 3","pages":"257 - 276"},"PeriodicalIF":1.2,"publicationDate":"2025-02-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143570985","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}

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Congress, Conferences, and Workshops

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-11 DOI: 10.1007/s10337-025-04395-7

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