Chromatographia最新文献_第5页

A Comprehensive Stability-indicating Method for Teriflunomide: Impurity Profiling and Degradation Analysis in Tablet Formulations 特立氟米特综合稳定性指示法：片剂中杂质分析与降解分析

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}

引用次数: 0

Stability-Indicating RP-HPLC Method for the Quantification of Daprodusdat in Pharmaceutical Formulation 稳定性指示反相高效液相色谱法定量测定药物制剂中药效学成分

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 感谢我们2024年的审稿人

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 设计与绿色化学相结合的可持续药物开发：阿卡拉替尼稳定性研究

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 大会、会议和讲习班

IF 1.2 4区化学

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

引用次数: 0

Effects of Porous Structure of Separation Column on Chromatograms Obtained by Phase-Separation Mode in HPLC 分离柱的多孔结构对HPLC相分离方式色谱图的影响

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-10 DOI: 10.1007/s10337-025-04392-w

Tetsuro Katayama, Takeshi Iharada, Yuki Obata, Hiroshi Sakamaki, Kazuhiko Tsukagoshi

{"title":"Effects of Porous Structure of Separation Column on Chromatograms Obtained by Phase-Separation Mode in HPLC","authors":"Tetsuro Katayama, Takeshi Iharada, Yuki Obata, Hiroshi Sakamaki, Kazuhiko Tsukagoshi","doi":"10.1007/s10337-025-04392-w","DOIUrl":"10.1007/s10337-025-04392-w","url":null,"abstract":"<div><p>A novel HPLC system utilizing a phase-separation multiphase flow as the eluent has been developed, referred to as phase-separation mode. This research explores the influence of the porous structure in an octadecyl-modified silica (ODS) column (with a pore diameter of 12 nm) on chromatographic outcomes under the phase-separation mode in HPLC. The chromatograms obtained from the porous ODS column were compared to those generated with a non-porous ODS column. In preliminary experiments, twenty-four mixed solutions, comprising combinations of water/acetonitrile/ethyl acetate and water/acetonitrile, were introduced as eluents at a column temperature of 20 °C. A model mixture of 2,6-naphthalenedisulfonic acid (2,6-NDS) and 1-naphthol (1-NA) was injected into the system, with separation achieved in most solutions except for some highly organic solvent-rich solutions where 2,6-NDS eluted faster than 1-NA, indicating reverse-phase mode operation. Subsequently, the separation of the model mixture was assessed at 0 °C, and four specific ternary mixtures were analyzed in detail at both 20 °C and 0 °C. These ternary mixtures, defined by their volume ratios, exhibited a two-phase separation, establishing a phase-separation multiphase flow. Consequently, the solution flow was homogeneous at 20 °C and heterogeneous at 0 °C. For instance, solutions with water/acetonitrile/ethyl acetate ratios of 20:60:20 (organic solvent-rich) and 70:23:7 (water-rich) were introduced as eluents at both 20 °C and 0 °C. At 0 °C in the organic solvent-rich eluent, 1-NA eluted faster than 2,6-NDS, characteristic of the phase-separation mode. In contrast, the water-rich eluent resulted in faster elution of 2,6-NDS at both temperatures. The porous ODS column displayed improved separation efficiency at 0 °C compared to the non-porous column, which can be attributed to the porous effect under phase-separation conditions.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 3","pages":"215 - 224"},"PeriodicalIF":1.2,"publicationDate":"2025-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143571023","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

Quantification of Seven Known and Several Unknown Impurities from Fluticasone Furoate and Oxymetazoline Hydrochloride Nasal Spray Product Using RP-HPLC UV Methodology RP-HPLC - UV法定量测定糠酸氟替卡松盐酸羟甲唑啉鼻喷雾剂中7种已知和几种未知杂质

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-10 DOI: 10.1007/s10337-025-04390-y

Shrikant V. Kulkarni, Surbhi Lokhande, Bhaskar D. Musmade, Shrinivas G. Bhope, Mitesh Nagar, Sharad P. Panchgalle, Vijaykumar S. More

{"title":"Quantification of Seven Known and Several Unknown Impurities from Fluticasone Furoate and Oxymetazoline Hydrochloride Nasal Spray Product Using RP-HPLC UV Methodology","authors":"Shrikant V. Kulkarni, Surbhi Lokhande, Bhaskar D. Musmade, Shrinivas G. Bhope, Mitesh Nagar, Sharad P. Panchgalle, Vijaykumar S. More","doi":"10.1007/s10337-025-04390-y","DOIUrl":"10.1007/s10337-025-04390-y","url":null,"abstract":"<div><p>Combination nasal spray products containing fluticasone furoate and oxymetazoline hydrochloride are commonly used to treat asthma, chronic pulmonary diseases, and perennial allergic rhinitis. However, testing for impurities in pharmaceutical products is a challenging task due to the similarity in properties between the impurities and the drugs. It is important to strictly maintain the product safety and quality to ensure the regulatory compliance. An attempt has been made to develop and validate a new simple, single-run RP-HPLC method for the simultaneous estimation of seven known and several unknown impurities from fluticasone furoate and oxymetazoline hydrochloride nasal spray products<b>.</b> The separation of multiple impurity peaks was achieved by using a 5 µm, Inertsil ODS 3 V, 250 × 4.6 mm column. Dual-wavelength UV detector (220 nm and 240 nm) was used for the detection of oxymetazoline hydrochloride, fluticasone furoate and their impurities. The relative response factor was calculated for all the known impurities to make the method accurate, simple and economical. The developed method was validated following the guidelines outlined in the ICH Q2(R2). The forced degradation study results confirmed the stability-indicating nature of the method. The developed impurity profiling methodology will greatly help the quality control labs in maintaining the safety and efficacy of finished products and to comply with the regulatory requirements of various countries. Overall, the proposed method offers unparalleled precision, accuracy, sensitivity, and cost-effectiveness making it a valuable addition to the pharmaceutical industry.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 3","pages":"243 - 255"},"PeriodicalIF":1.2,"publicationDate":"2025-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143571024","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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Isolation and Purification of Isoflavones and Isoflavone Glycosides from Dalbergia sissoo Leaves and In silico Evaluation for Anti-aging Potential 黄檀叶中异黄酮和异黄酮苷的分离纯化及抗衰老潜力的硅评价

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-09 DOI: 10.1007/s10337-025-04388-6

Vallabh Mulay, Arun Kumar Balasubramaniam, Ganesh Saste, Siddharth J. Modi, Ritu Trivedi, Lal Hingorani

{"title":"Isolation and Purification of Isoflavones and Isoflavone Glycosides from Dalbergia sissoo Leaves and In silico Evaluation for Anti-aging Potential","authors":"Vallabh Mulay, Arun Kumar Balasubramaniam, Ganesh Saste, Siddharth J. Modi, Ritu Trivedi, Lal Hingorani","doi":"10.1007/s10337-025-04388-6","DOIUrl":"10.1007/s10337-025-04388-6","url":null,"abstract":"<div><p><i>Dalbergia sissoo</i> Roxb., rich in isoflavones and isoflavone glycosides, is widely used to treat osteogenic effects, pain, and other diseases. This study employed simple procedures based on preparative reversed-phase high-pressure liquid chromatography (prep-RP-HPLC) for large-scale isolation of isoflavones and isoflavone glycosides present in <i>Dalbergia sissoo</i> leaves (DSL). The seven compounds were isolated from the ethanolic extract by the preparative HPLC–PDA method, and their purity was > 95%. The authors carried out an in silico analysis to find possible anti-aging compounds. Isolated compounds biochanin-A-7-O-[β-Dapiofuranosyl-(1–5)-β-D-apiofuranosyl-(1–6)-β-D-glucopyranoside (DS2) and biochanin-A-7-O [β-D-apiofuranosyl-(1–6)-β-D-glycopyranoside (DS3) demonstrated docking scores of −10.466 and −9.430 with docking energies of -81.864 and -77.531 kcal/mol, respectively, to the Hyaluronidase enzyme. For the Collagenase enzyme, they showed docking scores of −10.734 and −10.777 with docking energies of −107.102 and −98.317 kcal/mol, respectively. Against the Tyrosinase enzyme, Compounds DS2 and DS3 had docking scores of −7.333 and −7.993 with docking energies of −59.933 and −84.825 kcal/mol, respectively. For the elastase enzyme, they exhibited docking scores of −9.840 and −7.993 with docking energies of −68.490 and −84.815 kcal/mol, respectively. This study found that the isolation and purification method is simple and produces neat chromatograms with good selectivity and reproducibility. At the same time, docking results revealed that the compounds exhibited anti-aging properties.</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":"193 - 203"},"PeriodicalIF":1.2,"publicationDate":"2025-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143570949","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

Effect of Sudan Black B on the Separation and Characterization of Serum Lipoproteins by Asymmetrical Flow Field-Flow Fractionation 苏丹黑B对不对称流场-流分馏法分离和表征血清脂蛋白的影响

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-08 DOI: 10.1007/s10337-025-04393-9

Chenjing Zhang, Xiaoyue Zhang, Kaiming Yang, Jing Zhang, Xiaodong Dong, Haiyang Dou

{"title":"Effect of Sudan Black B on the Separation and Characterization of Serum Lipoproteins by Asymmetrical Flow Field-Flow Fractionation","authors":"Chenjing Zhang, Xiaoyue Zhang, Kaiming Yang, Jing Zhang, Xiaodong Dong, Haiyang Dou","doi":"10.1007/s10337-025-04393-9","DOIUrl":"10.1007/s10337-025-04393-9","url":null,"abstract":"<div><p>Coronary artery disease (CAD) is a very common cardiovascular disease. Clinically, the content of low-density lipoprotein-cholesterol (LDL-C) is often used as a predictor of CAD. However, severe CAD has been observed in patients with normal level of LDL-C. In this study, the serum lipoproteins stained with Sudan Black B (SBB) were separated and characterized by using asymmetrical flow field-flow fractionation (AF4) coupled with ultraviolet visible (UV/Vis) detector (AF4-UV/Vis). The effects of SBB staining conditions and AF4 operation conditions on AF4 analysis of serum lipoproteins were systematically investigated. The membrane fouling was alleviated by adjusting SBB staining conditions, which enhances the repeatability and accuracy of AF4 analysis of serum lipoproteins. Moreover, the baseline separation of LDL and high-density lipoprotein (HDL) was obtained by AF4 under optimized operation conditions. The results showed that the LDL/HDL value of healthy people was lower than that of CAD patients. The results revealed that the combination of AF4-UV/Vis and SBB staining is a promising approach for the separation and characterization of serum lipoproteins, which is beneficial to screening potential predictors of CAD.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 4","pages":"345 - 354"},"PeriodicalIF":1.2,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143786486","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

Development and Validation of an HPLC Method for the Simultaneous Determination of Eight Related Substances in Fosaprepitant Dimeglumine API 同时测定Fosaprepitant二聚氨胺原料药中8种有关物质的高效液相色谱方法的建立与验证

IF 1.2 4区化学

Chromatographia Pub Date : 2025-02-06 DOI: 10.1007/s10337-025-04389-5

Zhiling Cao, Ling Zhang, Maolong Huang, Siyi Xia, Yuhan Sun, Xudong Yu, Dahua Shi, Jian Zhu, Fan Xu

{"title":"Development and Validation of an HPLC Method for the Simultaneous Determination of Eight Related Substances in Fosaprepitant Dimeglumine API","authors":"Zhiling Cao, Ling Zhang, Maolong Huang, Siyi Xia, Yuhan Sun, Xudong Yu, Dahua Shi, Jian Zhu, Fan Xu","doi":"10.1007/s10337-025-04389-5","DOIUrl":"10.1007/s10337-025-04389-5","url":null,"abstract":"<div><p>The purpose of this study was to develop and validate a robust, precise, and selective high-performance liquid chromatography (HPLC) method for the separation and determination of related impurities in fosaprepitant dimeglumine API. The chromatographic separation was performed on a Supersil ODS-2 column (250 × 4.6 mm, 5 µm) at a wavelength of 215 nm using a mixture of phosphate buffer (pH 2.15) and acetonitrile as the mobile phase in gradient elution mode. The validation results demonstrate that the method exhibits acceptable specificity, linearity, accuracy, precision, and robustness. The detection limits and quantitation limits ranged from 1.5 to 12.5 ng mL<sup>−1</sup> and from 3.0 to 37.5 ng mL<sup>−1</sup>, respectively. A linear relationship was observed between the peak area and concentration of fosaprepitant and its eight related impurities with a correlation coefficient value of <i>r</i><sup>2</sup> ≥ 0.999. The analysis of commercial fosaprepitant dimeglumine products revealed a significantly higher purity than expected, with all known impurities falling below specification limits. The new HPLC method has been successfully applied to analyze commercial bulk drug samples and is suitable for quality-control laboratories for both qualitative and quantitative assessment of eight related substances in the fosaprepitant dimeglumine API.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 3","pages":"205 - 214"},"PeriodicalIF":1.2,"publicationDate":"2025-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143570976","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