Journal of chromatographic science最新文献_第6页

Harmonized Approach of Design of Experiments with Green and White Analytical Chemistry in Unified Framework for Synchronous Chromatographic Assay of Diverse Combinations of Anti-diabetic Drugs in Pharmaceutical Dosage Forms. 药物剂型中不同组合抗糖尿病药物同步色谱分析统一框架中绿白分析化学实验设计的协调方法

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-08-30 DOI: 10.1093/chromsci/bmaf051

Pintu Prajapati, Bageshree Rana, Veerashakar Pulusu, Anzarul Haque, Shailesh Shah

{"title":"Harmonized Approach of Design of Experiments with Green and White Analytical Chemistry in Unified Framework for Synchronous Chromatographic Assay of Diverse Combinations of Anti-diabetic Drugs in Pharmaceutical Dosage Forms.","authors":"Pintu Prajapati, Bageshree Rana, Veerashakar Pulusu, Anzarul Haque, Shailesh Shah","doi":"10.1093/chromsci/bmaf051","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf051","url":null,"abstract":"Antidiabetic drugs, including metformin hydrochloride, are typically used to treat diabetes mellitus. Current methods for evaluating these drug combinations often involve the use of harmful solvents and specific conditions, leading to environmental risks and substantial toxic waste. White analytical chemistry proposes an innovative solution to this problem by developing environmentally friendly, cost-effective and user-friendly chromatographic methods. A synchronous chromatographic assay method for multiple combined pharmaceutical dosage forms of antidiabetic drugs was developed using a single set of chromatographic conditions and safe organic solvents. Method development was carefully carried out using a design of experiments approach to reduce organic solvent waste. The Plackett-Burman design was used in the screening phase to identify critical method variables and responses, facilitated by Minitab 18 software. The Box-Behnken design was then used to optimize these critical variables. A synchronous chromatographic assay of multiple combined pharmaceutical dosage forms was conducted under optimized chromatographic conditions. Finally, a thorough evaluation of the proposed and existing chromatographic methods was conducted using green and white analytical chemical metrics.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 8","pages":""},"PeriodicalIF":1.3,"publicationDate":"2025-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145185648","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

Simultaneous Bioanalytical Method Development and Validation of Navitoclax and Doxorubicin in Rat Plasma Using UHPLC-HESI-LTQ-MS. 用UHPLC-HESI-LTQ-MS建立大鼠血浆中纳维托昔和阿霉素的同时生物分析方法及验证。

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-08-30 DOI: 10.1093/chromsci/bmaf046

Nitesh Rai, Deepak Kumar, Parul Sharma, Pirangi Srikanth, Shaik Khaja Moinuddin, Pramod Kumar, Sukhendu Nandi

{"title":"Simultaneous Bioanalytical Method Development and Validation of Navitoclax and Doxorubicin in Rat Plasma Using UHPLC-HESI-LTQ-MS.","authors":"Nitesh Rai, Deepak Kumar, Parul Sharma, Pirangi Srikanth, Shaik Khaja Moinuddin, Pramod Kumar, Sukhendu Nandi","doi":"10.1093/chromsci/bmaf046","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf046","url":null,"abstract":"A simple, sensitive, and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was successfully developed and validated to determine navitoclax and doxorubicin in rat plasma. Ketoconazole and daunorubicin were employed as internal standards to ensure accurate quantification and method consistency. The sample preparation involved a straightforward protein precipitation technique, which facilitated efficient extraction of the analytes from the plasma matrix. The resulting supernatant was subjected to drying using a vacuum concentrator and later reconstituted before being injected into the LC-MS system. Separation was carried out using a SHIMADZU Shim-pack GIST C-18 column with mobile phase, consisting of a carefully balanced mixture of acetonitrile and water with 0.1% formic acid, with a flow rate of 0.5 mL/min. This composition ensured efficient elution and minimized matrix effects, contributing to the method's robustness and reproducibility. The developed method was comprehensively validated according to regulatory guidelines, assessing various parameters including specificity, selectivity, sensitivity, calibration curve performance, precision, accuracy, stability and dilution integrity. This bioanalytical method has the potential to be extended to various clinical settings, enabling the monitoring drug metabolism, monitoring potential drug-drug interactions and understanding the pharmacokinetic profile and adverse effect potential of the combination therapy.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 8","pages":""},"PeriodicalIF":1.3,"publicationDate":"2025-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144955817","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

Simultaneous Analysis of Cyproconazole and Tebuconazole in Suspension Concentrate Formulation by Reverse-Phase High-Performance Liquid Chromatography. 反相高效液相色谱法同时分析悬浮液中环丙康唑和戊康唑的含量。

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-08-30 DOI: 10.1093/chromsci/bmaf047

Sahadev Katam, Prasad Munipalli, Bhavani Balram, Vasu Govardhana Reddy Peddiahgari

引用次数: 0

Streamlined Sample Cleanup: Small Molecule Fractionation and Extraction Via Low-Volume Polymer Monolithic Columns for In-Line Analysis. 流线型样品清理：小分子分离和提取通过小体积聚合物整体柱进行在线分析。

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-08-30 DOI: 10.1093/chromsci/bmaf049

Ischa Bremer, Charles Clark, Bert Wouters, Amy Harms, Thomas Hankemeier

{"title":"Streamlined Sample Cleanup: Small Molecule Fractionation and Extraction Via Low-Volume Polymer Monolithic Columns for In-Line Analysis.","authors":"Ischa Bremer, Charles Clark, Bert Wouters, Amy Harms, Thomas Hankemeier","doi":"10.1093/chromsci/bmaf049","DOIUrl":"10.1093/chromsci/bmaf049","url":null,"abstract":"Polymer monoliths are stationary-phase materials for liquid chromatography and solid-phase extraction. Their porous structure, tuneability and simple synthesis enable tailoring to specific analysis requirements in analytical chemistry. Typically, polymer monoliths are used to separate larger biomolecules. Due to their lower binding capacity, the applications of polymer monoliths for the chromatographic separation of small molecules remain limited. However, recent literature has shown that polymer monoliths have the potential for the extraction of small molecules. In this research, butyl methacrylate-co-ethylene glycol dimethacrylate polymer monoliths were synthesized using localized UV polymerization in capillaries. The performance of reversed-phase polymer monoliths in automated in-line solid-phase extraction-mass spectrometry was demonstrated by the analysis of endocannabinoids from neat standard mixes and spiked cell culture media without prior sample preparation. The synthesized monoliths exhibited a binding capacity of 1896 pmol. Furthermore, we showed the repeatability of the monolith synthesis, with a variance in permeability of 19%. The system's stability is demonstrated through the analysis of multiple batches, comparing different monoliths and reusing the same monolith repeatedly, resulting in relative standard deviations (RSDs) below 20% for all extracted compounds. This automated method with hyphenated mass spectrometry improves throughput over previous manual monolithic extractions for small molecules.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 8","pages":""},"PeriodicalIF":1.3,"publicationDate":"2025-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144955879","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

Method for Simultaneous Determination of Amino Acid Surfactants Sodium N-Lauroylsarcosinate and Sodium Methyl Cocoyl Taurate in Personal Care Products, by Using High Performance Liquid Chromatography. 高效液相色谱法同时测定个人护理用品中氨基酸表面活性剂n -月桂酰肌氨酸钠和甲基椰油酰牛磺酸钠的含量。

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-07-24 DOI: 10.1093/chromsci/bmaf044

Kumar Thangarathinam, Udhayachandran Narayanan

引用次数: 0

Optimized Simultaneous Estimation of Metformin, Teneligliptin, and Pioglitazone in Tablet and Bulk Drug: A Box-Behnken Design Approach for RP-UFLC Method Development and Validation. 片剂和原料药中二甲双胍、替尼格列汀和吡格列酮含量的优化同时估计：RP-UFLC方法开发与验证的Box-Behnken设计方法

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-07-24 DOI: 10.1093/chromsci/bmaf045

Jignesh Panchal, Jayesh Dhalani

{"title":"Optimized Simultaneous Estimation of Metformin, Teneligliptin, and Pioglitazone in Tablet and Bulk Drug: A Box-Behnken Design Approach for RP-UFLC Method Development and Validation.","authors":"Jignesh Panchal, Jayesh Dhalani","doi":"10.1093/chromsci/bmaf045","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf045","url":null,"abstract":"The combination of metformin (MET), teneligliptin (TEN), and pioglitazone (PIO) is newest fixed-dose combination for the treatment type 2 diabetes launched in India. An accurate, rapid, and cost-effective reversed phase ultra-fast liquid chromatography method was developed, validated, and applied for the quantification of MET, TEN, and PIO in bulk and tablet with a very short runtime. Box-Behnken design was implemented to optimize the ultra-fast liquid chromatography conditions. A C18 column (150 × 4.6 mm, 5μ) was utilized with a mobile phase buffer (0.01 M phosphate buffer, pH = 6.2) and acetonitrile in a 51:49 ratio with flow rate of 1.5mL/min at column oven temperature 40°C. Detection was carried out at 255nm by 20 μL injection volume. Retention times were found to be 0.94, 1.36, and 2.07 min, whereas the limit of quantification were 0.209, 0.712, and 57.030 μg/mL for MET, TEN, and PIO, respectively. The linearity of anticipated development was studied in the range of 250-1250 μg/mL (MET, r2 = 0.99974), 10-50 μg/mL (TEN, r2 = 0.99997), and 7.5-37.5μg/mL (PIO, r2 = 0.99999). The relative standard deviation values for method and intermediate precision were <2%. The method was validated as per International Conference on Harmonization guideline for accuracy, precision, linearity, limit of detection, limit of quantification, specificity, robustness, and forced degradation. This is the only study that presents reversed phase ultra-fast liquid chromatography method for the new fixed-dose combination of MET, TEN, and PIO, with the shortest run time of 3.0 min. The proposed method is innovative, efficient, precise, quickest, and economical with high accuracy which makes the study novel.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 7","pages":""},"PeriodicalIF":1.3,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144955846","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

Screening Method for the Determination of per- and Polyfluoroalkyl Substances (PFAS) in Textiles by Combustion and Ion Chromatography. 燃烧和离子色谱法测定纺织品中全氟烷基和多氟烷基物质的筛选方法。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-07-24 DOI: 10.1093/chromsci/bmaf043

Lihua Cao, Youchao Ding, Kai Qian, Xiangxiang Wang, Xiaoqiong Wang, Jia Zhou, Juan Tang

{"title":"Screening Method for the Determination of per- and Polyfluoroalkyl Substances (PFAS) in Textiles by Combustion and Ion Chromatography.","authors":"Lihua Cao, Youchao Ding, Kai Qian, Xiangxiang Wang, Xiaoqiong Wang, Jia Zhou, Juan Tang","doi":"10.1093/chromsci/bmaf043","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf043","url":null,"abstract":"A screening method was developed for the determination of per- and polyfluoroalkyl substances in textiles by combustion and ion chromatography. In this work, a new type of high-temperature combustion absorption device was designed, and the samples were burned, cracked and gasified by temperature programmed heating mode. The produced free fluorine and hydrogen fluoride gases were absorbed by water vapor and completely transformed into inorganic fluoride anion. After condensation and collection, it was separated and determined by ion chromatography. The pre-treatment conditions were optimized including the sample weight, the combustion method, the combustion gas and its flow rate, the water evaporation rate and the condensate collection method. Method validation was performed in negative samples of cotton, wool and polyester, at spiked levels of 5, 50 and 200 mg/kg, respectively. The average recoveries were between 85.7 and 95.0% with relative standard deviations <20% (n = 7) indicating satisfactory accuracy and repeatability. The calibration curve was performed with the correlation coefficients (R2) higher than 0.999 within a linearity range of 0.01-2.0 mg/L. The limit of quantification was 5.0 mg/kg. The developed method was successfully used to determine the total fluorine in market samples. It can meet the screening determination of PFAS in various textiles.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 7","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144707649","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

Plasticizers Analysis in Extractables and Leachables by Gas Chromatography-Mass Spectrometry with Parallel Polyarc®/Flame Ionization Detector. 用平行多弧/火焰电离检测器的气相色谱-质谱法分析可萃取物和可浸物中的增塑剂。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-06-10 DOI: 10.1093/chromsci/bmaf034

Jianxin Yu, Scott Citrowske, Jacob Strange, Nikki Carlson, Jeannette Polkinghorne

{"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":"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.","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}

引用次数: 0

AQbD-Based Development and Validation of HPTLC Method for Simultaneous Determination of Glycopyrronium, Formoterol Fumarate and Budesonide in Rotacaps. 基于aqbd的高效薄层色谱法同时测定罗盘菜中甘霉素、富马酸福莫特罗和布地奈德含量的建立与验证。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-06-10 DOI: 10.1093/chromsci/bmaf033

Dharati R Saradhara, Vijaykumar K Parmar

{"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":"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.","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}

引用次数: 0

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. 超声真空辅助顶空固相微萃取法测定药品中溶剂残留量及其与传统顶空固相微萃取法的比较

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-06-10 DOI: 10.1093/chromsci/bmaf039

Somayeh Hajipour, Alireza Ghiasvand, Mohammad Hajipour

{"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":"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.","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}

引用次数: 0