Journal of chromatographic science最新文献

{"title":"Plasticizers Analysis in Extractables and Leachables by Gas Chromatography-Mass Spectrometry with Parallel Polyarc®/Flame Ionization Detector.","authors":"Jianxin Yu, Scott Citrowske, Jacob Strange, Nikki Carlson, Jeannette Polkinghorne","doi":"10.1093/chromsci/bmaf034","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf034","url":null,"abstract":"<p><p>Plasticizers such as phthalate acid esters including di-(2-ethylhexyl) phthalate (DEHP) and its alternatives are commonly found in extractables and leachables (E&Ls) from plastic-based medical devices. Regulatory agencies require manufacturers to monitor, qualify and quantify the E&Ls from medical devices to ensure the safety. Analyzing E&Ls from medical devices is difficult due to the unpredictability and complexity of matrices. The advent of the novel Polyarc/Flame Ionization Detector (FID), which features compound-independent response, provides the opportunity of quantitation of unknowns-to-be-identified E&Ls without using pure substances for establishing calibration. The present work evaluated firstly the feasibility and efficacy of full scan GC-MS with parallel Polyarc/FID system through analysis of plasticizers in E&Ls. In the same injection, E&Ls were identified by full scan GC-MS, then quantified through Polyarc/FID response factor of internal standards. The results showed that quantitation via response factor from internal standards are more accurate so the need for standards of the identified E&Ls is eliminated. The method can combine screening process and target analysis into a one-step execution, which makes it desirable for E&L analysis. The method was applied to a polyvinyl chloride medical device, yielding 1.183 g/device of acetyl tri-n-butyl citrate, 370.2 mg/device of trioctyltrimellitate, and 3.068 mg/device of DEHP.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144325895","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":"AQbD-Based Development and Validation of HPTLC Method for Simultaneous Determination of Glycopyrronium, Formoterol Fumarate and Budesonide in Rotacaps.","authors":"Dharati R Saradhara, Vijaykumar K Parmar","doi":"10.1093/chromsci/bmaf033","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf033","url":null,"abstract":"<p><p>Analytical quality by design was used to develop and validate a sensitive, accurate and precise high performance thin layer chromatography method for the determination of glycopyrronium (GLY), formoterol fumarate (FFD) and budesonide (BUD) in pharmaceutical dosage form (Rota caps). Design of Experiment was carried out by Placket-Burman screening design and Box- Behnken response surface methodology using peak area and Rf value as critical method attributes. Method operable design region was navigated for optimization and development of the method. The developed method was validated as per ICH Q2 guidelines. Linearity was found to be 0.25-1.25 μg/band, 0.12-0.60 μg/band and 4-20 μg/band respectively for GLY, FFD and BUD. Accuracy of the method was determined by recovery studies where the percentage recoveries were found to be 98-101%. The precision of the method was determined by repeatability and intermediate precision studies. The % RSD values were found to be less than 2, proving method was precise. The method was found specific and precise for the estimation of drugs. The developed method was applied for the assay of rotacaps and results were found in good agreement with the label claim.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144317008","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 of a Novel Ultrasound Vacuum-Assisted Headspace Solid-Phase Microextraction Approach for Determination of Solvent Residuals in Pharmaceuticals and Comparison with Traditional Headspace Solid-Phase Microextraction Method.","authors":"Somayeh Hajipour, Alireza Ghiasvand, Mohammad Hajipour","doi":"10.1093/chromsci/bmaf039","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf039","url":null,"abstract":"<p><p>In this report, an ultrasonication and vacuum-assisted headspace solid-phase microextraction procedure followed by gas chromatography-flame ionization detection (UVA-HS-SPME-GC-FID) was proposed for direct extraction of solvent residuals, including benzene, toluene, ethyl benzene, m,p-xylene and o-xylene, in pharmaceutical matrices. A novel robust, reliable and durable nanocomposite solid-phase microextraction (SPME) fiber was prepared by layer-by-layer coating of 3-aminopropyltriethoxysilane-functionalized graphene on a stainless-steel wire. Then, the proposed fiber was used for headspace SPME and trapping of toluene as a residual solvent in solid penicillin, ampicillin and cefazolin vials followed by gas chromatography-flame ionization detection. UVA-HS-SPME-GC-FID achieves better validation parameters, including the limit of detection, limit of quantification, linearity, recovery and repeatability, in comparison with conventional HS-SPME-GC-FID. The UVA-HS-SPME-GC-FID strategy is very effective for quantitatively tracing volatile and semivolatile solvent residuals in various pharmaceutical drugs.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144560187","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":"Simple, Sensitive and Reproducible High-performance Liquid Chromatographic Method for Determination of Mixed Tocotrienol in Blood Plasma using Fluorescent Detection.","authors":"Teong G Thor, Song T Goh, Kah H Yuen, Jacqueline K K Mark, Siok Y Chan","doi":"10.1093/chromsci/bmaf041","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf041","url":null,"abstract":"<p><p>A simple, sensitive and reproducible high-performance liquid chromatographic (HPLC) method with fluorescence detection was developed and validated for the simultaneous quantification of mixed tocotrienols (α-, γ- and δ-) in human plasma. The method involves a straightforward sample preparation step, where plasma samples are deproteinized using a mixture of acetonitrile and tetrahydrofuran (3:2, v/v), followed by direct injection into the HPLC system. Separation was achieved using a methanol mobile phase at a flow rate of 1.5 mL/min, with fluorescence detection at excitation and emission wavelengths of 296 nm and 330 nm, respectively. The method demonstrated excellent linearity over concentration ranges of 12.7 ng/mL to 2.54 μg/mL for α-tocotrienol, 19.2 ng/mL to 3.84 μg/mL for γ-tocotrienol and 4.6 ng/mL to 0.923 μg/mL for δ-tocotrienol, with quantification limits of 12.7 ng/mL, 19.2 ng/mL and 4.6 ng/mL, respectively. Recovery rates ranged from 85.0% to 111.2%, and both intra-day and inter-day precision showed relative standard deviations below 15%. The method was validated for accuracy, precision and stability under various conditions, including freeze-thaw cycles and long-term storage. This HPLC method offers a rapid, sensitive and reliable approach for quantifying tocotrienols in human plasma, making it suitable for preclinical and clinical studies, particularly in pharmacokinetic and bioavailability research.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144591305","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":"Simultaneous Measurement of Mycophenolic Acid with Other Immunosuppressants in Whole Blood and Plasma by Using Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Yu-Ping Wang, Xiao-Hui Zhai, Xi-Han Wang, Kun Shao, Pei-Jun Zhou, Hao-Qiang Shi, Bing Chen","doi":"10.1093/chromsci/bmaf037","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf037","url":null,"abstract":"<p><p>Therapeutic drug monitoring (TDM) of immunosuppressive drugs (ISDs) is essential for transplant recipients. The aim of this study is to establish an LC-MS/MS method to determine mycophenolic acid (MPA) and its metabolite, cyclosporin A (CsA), tacrolimus (TAC) and sirolimus (SRL) levels in whole blood and plasma simultaneously. Whole blood and plasma samples were treated with protein precipitation. After centrifugation, the supernatant was eluted through Agilent Eclipse XDB-C18 (3.5 μm, 2.1 mm × 100 mm) column by water (2 mmol/L ammonium formate) and methanol through a gradient method. The ISDs in renal allograft recipients were compared with TDM results. The methods established were linear within a range of 0.204-51 μg/mL for MPA, 2.0-500 μg/mL for MPAG, 4-1,000 ng/mL for CsA, 0.2-50 ng/mL for TAC and 0.2-50 ng/mL for SRL (r2 = 0.9998) in plasma and whole blood. The intra- and inter-day accuracy was in the range of 85-115%, and imprecision of all ISDs was <15%. Plasma MPA and MPAG levels can be estimated based on whole blood level: Cplasma = 1.52 × Cblood + 0.16 (r2 = 0.9168) and Cplasma = 1.58 × Cblood - 0.56 (r2 = 0.9069). The CsA (r2 = 0.9694, n = 60), TAC (r2 = 0.9426, n = 115) and SRL (r2 = 0.9484, n = 70) levels in whole blood were consistent with those obtained from the immunoassays. The LC-MS/MS method established is suitable for patients with various immunosuppressive regimens.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144484501","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 Development of Piperine as Herbal Reference Material from Black Pepper for Quality Control Purposes: Liquid Chromatography-Quadrupole Time-of-Flight, Nuclear Magnetic Resonance, and Thermal Analysis.","authors":"Swati Ramesh Pawar, Sachin Dattram Pawar, Sandeep Jat, Rashinikumar Samandram, Dnyaneshwar Maykar, Pratik Gore, Pramod Kumar","doi":"10.1093/chromsci/bmaf036","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf036","url":null,"abstract":"<p><p>Various spices and their oleoresins are being marketed since long and it has multibillion market. One of the most often used spices is black pepper (Piper nigrum), which gets its pungent flavour from volatile chemical components, essential oils, and an alkaloid called piperine. Piperine is also known for huge therapeutic benefits and most people are using daily in food products also. Most significantly, piperine is recognised as a bioavailability enhancer by stopping CYP enzyme activity. Therefore, our aim is to develop black pepper extract and isolation of piperine from black pepper. Various analytical techniques including, UV-Visible Spectroscopy, Fourier Transform Infrared Spectroscopy, Differential Scanning Calorimetry, Thermogravimetric Analysis, Proton Nuclear Magnetic Resonance, Carbon-13 Nuclear Magnetic Resonance, High-Resolution Mass Spectrometry were used to characterize piperine. NMR confirms its structure and molecular weight was confirmed by HRMS. Purified piperine has shown HPLC purity >99.5%. DSC has shown the melting peaks of 130.12°C. Piperine have great commercial potential as reference materials for regular quality control in the herbal industries for black pepper-based products.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144626428","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":"Quantitation of Catechin, Epicatechin, Quercetin and Kaempferol by Liquid Chromatography with Diode Array Detection and Friedelin by Gas Chromatography Coupled to Mass Spectrometry in Maytenus ilicifolia Mart. ex Reiss Extracts.","authors":"Sara Batista do Nascimento, Maria José Nunes de Paiva, Sumaia Araújo Pires, Whocely Victor de Castro, Isabela Costa César","doi":"10.1093/chromsci/bmaf040","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf040","url":null,"abstract":"<p><p>Maytenus ilicifolia Mart. ex Reiss (espinheira-santa) is a plant native to South America, popularly used in the treatment of gastric disorders. A liquid chromatographic (LC) method was developed using a C18 column and mobile phase composed of acetonitrile and 0.02% (v/v) trifluoracetic acid using gradient elution. Ultraviolet detection was performed at 270 and 369 nm. Gas chromatography coupled to mass spectrometry (GC-MS) analysis was performed using a DB-5MS column and helium as mobile phase. Five samples of M. ilicifolia extracts were assayed by both methods, which were fully validated. Using the LC method, the quantified levels varied from 0.06 to 0.49% (w/w) for catechin and from 0.10 to 0.79% (w/w) for epicatechin. The maximum content of quercetin and kaempferol were 0.01 and 0.004% (w/w), respectively. Friedelin was quantified only in the hydroacetonic extract (0.98% w/w), by GC-MS. Both chromatographic methods showed to be reliable tools for the screening and quantitation of the main vegetal markers in M. ilicifolia herbal products.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144540404","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":"Comprehensive Profiling of the Chemical Constituents in Dioscorea Bulbifera Using High Performance Liquid Chromatography Coupled to Electrospray Ionization and Quadrupole Time-of-Flight Mass Spectrometry.","authors":"Qing Zhang, Jiasi Huang, Na Hu, You Peng, Zhiqiang Lei, Yun Ling","doi":"10.1093/chromsci/bmaf038","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf038","url":null,"abstract":"<p><p>The rhizome of Dioscorea bulbifera (RDB) has been used in folk and traditional Chinese medicine for the treatment of thyroid diseases and cancer. However, the chemical constituents are not fully clear. In this study, high-performance liquid chromatography coupled to electrospray ionization and quadrupole time-of-flight mass spectrometry was successfully used for the comprehensive characterization of chemical constituents in RDB. As a result, a total of 40 compounds were identified in RDB by comparison with the authentic standards or reported references, including 13 flavonoids, 2 diterpenoids, 2 stilbenoids, 12 steroidal saponins, and 11 phenolic derivatives. This study comprehensively elucidated the chemical basis of RDB and provided a robust foundation for the quality control and pharmacology research in the future.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144560186","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":"Quantitative Analysis of Ginkgo biloba Extracts Using a New HPLC Method: Single Standard for the Determination of Multiple Components.","authors":"Jianing Li, Ping Li, Hao Sun, Fan He, Qi Wu, Zhaofang Liu, Shuhong Ye, Yan Ding","doi":"10.1093/chromsci/bmaf032","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf032","url":null,"abstract":"<p><p>In this study, a quality control method utilizing high-performance liquid chromatography has been developed to simultaneously determine the content of 12 major flavonoids in Ginkgo biloba leaf (GBL) through fingerprint analysis and a single standard for the determination of multiple components (SSDMC). Thirteen batches of GBL samples and standardized extracts were analyzed using the SSDMC, traditional external standard (ES) and Chinese pharmacopoeia (CP) methods. The new quality control method was credible and feasible, having been sufficiently validated for linearity (r2 > 0.9993), limits of detection (0.13-0.83 μg/mL), limits of quantification (0.43-2.76 μg/mL), precision (relative standard deviation [RSD] < 0.89%), accuracy (92-114%, RSD < 1.76%), repeatability (RSD < 1.92%) and stability (RSD < 1.96%). The flavone contents observed in the 13 batches of GBL samples and standardized extracts showed no significant difference when using SSDMC and ES methods, and their contents were slightly higher than those obtained using the CP method.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144266361","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":"Phytochemical Profiling, Isolation, Characterization and Quantification of Triterpenoids from Terminalia Arjuna: A Multi-Location Study Using HPLC and Statistical Analyses.","authors":"Radhika Khanna, Gaurav Pandey, Santan Barthwal, Harish Singh Ginwal, Vinay Kumar Varshney","doi":"10.1093/chromsci/bmaf042","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf042","url":null,"abstract":"<p><p>Terminalia arjuna is a widely recognized medicinal tree known for its diverse pharmacological properties, particularly its cardioprotective effects. This study aimed to quantify two key bioactive triterpenoids, arjungenin and arjunic acid, in T. arjuna bark samples collected from 16 different geographical locations. A validated High-Performance Liquid Chromatography method was developed, demonstrating high precision, accuracy and sensitivity for the simultaneous quantification of these compounds. Statistical analyses, including Hierarchical Cluster Analysis, Principal Component Analysis and heat map visualization, were employed to classify populations based on their phytochemical composition. The results revealed significant variations in arjungenin and arjunic acid content among different populations, with the highest concentrations observed in samples from Amangarh tiger reserve (Bijnor) and Gorakhpur Forest division (Pharenda). These findings were further confirmed by ANOVA and Tukey's post hoc test. Additionally, variations in yield and total tannin content were observed, suggesting that environmental factors play a crucial role in secondary metabolite biosynthesis. The identification of high-yielding populations highlights the potential for targeted conservation efforts and the selection of superior genetic resources for pharmaceutical and nutraceutical applications. This study provides a comprehensive phytochemical assessment of T. arjuna populations and establishes a reliable analytical method for quality control and standardization. The findings contribute valuable insights into the influence of environmental factors on metabolite production, paving the way for future research on genetic and biochemical pathways regulating triterpenoid biosynthesis in T. arjuna. Moreover, flash chromatography was employed to isolate arjunic acid, and its structure was further validated using 1H-NMR and 13C-NMR spectroscopy, reinforcing the analytical accuracy of the method.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144591304","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}