{"title":"Application of Polydopamine-Based Magnetic Solid-Phase Extraction for Highly Sensitive Determination of Aristolochic Acid I from Traditional Chinese Medicine Samples.","authors":"Huimin Li, Huina Cao, Zixin Zhang, Fei Tian, Yi Zhang, Lijie Wu","doi":"10.1093/chromsci/bmae055","DOIUrl":"10.1093/chromsci/bmae055","url":null,"abstract":"<p><p>A low cost-effective and simple synthesis method combining magnetic solid-phase extraction (MSPE) and high-pressure liquid chromatography was developed for the analysis of aristolochic acids I (AAI) in traditional Chinese medicine samples. A novel polydopamine (PDA) modified magnetic nanoparticles with one single carbon layer (Fe3O4@1C NPs) via one-pot hydrothermal approach was prepared and then successfully employed to extract AAI for the first time. Dopamine (DA) can form a PDA layer on Fe3O4@1C NPs surface through self-polymerization to form Fe3O4@1C@PDA. As a surface modifier of DA, PDA offered more adsorption sites to AAI due to π-π stacking, hydrogen bonding and electrostatic interactions. The parameters of MSPE were optimized by univariate and multivariate methods (Box-Behnken design) in detail. High degree of linearity was obtained in the range of 0.05-200.0 μg/mL. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.08 and 0.25 μg/mL, respectively. The recoveries of AAI in spiked Xiaoqinglong mixture samples were in the range of 86.7 to 108.5% with the relative standard deviation of less than 5.2%. Thus, a fast, convenient, sensitive and eco-friendly method was successfully proposed and became a promising approach for the determination of AAI in herbal plants or its preparation in the manufacturing procedure.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142545731","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}
Rabab M Soliman, Yasmin Rostom, Yasmin M Fayez, Nadia M Mostafa, Hany H Monir
{"title":"Novel Green Chromatographic Approaches for Estimation of a Triple Common Cold Pharmaceutical Combination.","authors":"Rabab M Soliman, Yasmin Rostom, Yasmin M Fayez, Nadia M Mostafa, Hany H Monir","doi":"10.1093/chromsci/bmae050","DOIUrl":"10.1093/chromsci/bmae050","url":null,"abstract":"<p><p>Nowadays, there is a strong interest in the scientific community in developing innovative methodologies within a green analytical chemistry framework. Herein, we introduce the first chromatographic approaches for the concurrent estimation of paracetamol (PAR), carbinoxamine (CRX), and pseudoephedrine (PSE) intended to relieve COVID-19 and common cold symptoms. The first method was thin layer chromatography (TLC) densitometry, which depends on the separation of the studied medications on TLC silica gel plates using ethyl acetate: methanol: ammonia (7.0: 3.0: 0.2, by volume) as the developing system, and were scanned at 208.0 nm. The data were linear in the ranges of 1-25 μg/band for PAR, 1-25 μg/band for PSE and 0.1-5 μg/band for CRX. The second method was reversed-phase high-performance liquid chromatography separation on a Kromasil C18 column using a mixture of 0.01 M phosphate buffer containing 0.1% triethylamine (pH 3.5) adjusted with orthophosphoric acid and ethanol at a flow rate of 1.0 mL/min in a gradient program. The separated peaks were detected at 215.0 nm over a concentration range of 10-250 μg/mL for PAR, 5-35 μg/mL for PSE, and 0.5-25 μg/mL for CRX. Both approaches were validated according to International Conference on Harmonization (ICH) guidelines. Finally, the impact of these methods on the environment was evaluated by many tools.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142347577","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 and Validation of Rapid and Cost-Effective RP-HPLC/UV Method for Determination of Cetirizine/Levocetirizine in Blood Plasma of Smokers and Non Smokers: a Two Cohort Comparative Study.","authors":"Mashal Khattak, Zafar Iqbal, Asif Jan, Niaz Ali, Fazli Nasir, Naila Shahbaz","doi":"10.1093/chromsci/bmae058","DOIUrl":"10.1093/chromsci/bmae058","url":null,"abstract":"<p><p>In this research study, a simple, rapid, sensitive, and cost-effective Reverse Phase High Performance Liquid Chromatography method was developed and validated for determination of Cetirizine and Levocetirizine in human plasma. The drugs were separated on an ACE Generix100-5 C18 RP (250 × 4.6 mm, 5 μm) column, using Acetonitrile and Distilled water pH 7 (59:41 v/v) as mobile phase with a flow rate of 1.5 mL/min, retention time of 3.39 ± 0.02 min, detection wavelength of 230 nm, and column oven temperature at 26°C. The drug was extracted from human plasma using Methanol, the percent recovery was 97%. The LOD and LOQ for Cetirizine and Levocetirizine were 0.5 ng and 1 ng. The method was linear over the concentration range of 0.5-1000 ng /mL for Cetirizine and Levocetirizine. The method was applied for analysis of drugs in plasma following oral administration of Cetirizine (10 mg) and Levocetirizine (5 mg) in smokers and nonsmokers of Pashtun ethnicity belonging from different districts of Khyber Pakhtunkhwa, Pakistan. The difference between Cetirizine plasma levels in smokers and non-smokers was significant with p -value 0.0279.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142621373","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}
Trupesh M Pethani, Monika Sangani, Param S Santoki
{"title":"Stability Indicating High Performance Liquid Chromatography Method Development, Validation, and Characterization of Forced Degradant Product by Liquid Chromatography-Mass Spectroscopy for Molnupiravir and Favipiravir.","authors":"Trupesh M Pethani, Monika Sangani, Param S Santoki","doi":"10.1093/chromsci/bmaf015","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf015","url":null,"abstract":"<p><p>Coronavirus disease 2019 (COVID-19) is a disease caused by a virus named SARS-CoV-2. It is very contagious and has quickly spread around the world. COVID-19 most often causes respiratory symptoms that can feel much like a cold, a flu, or pneumonia. Molnupiravir (MLP) and Favipiravir (FAV) are two recently approved drugs for the ongoing COVID-19 pandemic drug combination help to reduce antiviral load with less side effect. MLP and Favipiravir standards subjected to degradation under different stress condition like acidic, basic, oxidative, thermal, and photostability. The current study endeavors to identify and characterize the degradation products of MLP and Favipiravir using Liquid Chromatography-Mass Spectrometry (LC-MS). Method developed and validated as per International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use Guideline (ICH) Q2(R1). The high performance liquid chromatography separation was achieved using Phenomenex Gemini 5 μ C18 (250 mm × 4.6 mm, 5 μm) column using mobile phase A and mobile phase B (15: 85% V/V) and the composition of mobile phase A: 10 mM ammonium acetate and mobile phase B: Acetonitrile (ACN) and methanol 70:30% V/V. Injection volume of 10 μL with 1.0 mL/min flow rate. The detection wavelength was 275 nm and the study was performed at 40°C column temperature. Excellent linear relationship between peak area of MLP and Favipiravir concentration in the range of 5-500 μg/mL for both drugs has been observed R2 = 0.9995 and R2 = 0.9996, respectively. Precision, accuracy, and robustness were found to be < 2% in terms of Relative Standard Deviation (RSD) and all other parameter were found within the specified criteria as per ICH guidelines. Proposed method has been successfully applied for quantification of MLP and Favipiravir in the presence of its impurities.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730260","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":"Fast Determination of Propofol in Human Plasma Using C18-Functionalized Magnetic Nanomaterials Followed by Supercritical Fluid Chromatography.","authors":"Shan-Yan Liang, Xiao-Min Xu, Peng Wang, Ming-Li Ye, Shui-Feng Zhang, Yong-Gang Zhao","doi":"10.1093/chromsci/bmae053","DOIUrl":"10.1093/chromsci/bmae053","url":null,"abstract":"<p><p>Novel C18-functionalized magnetic nanomaterials; i.e., C18@poly-styrene-divinylbenzene-glycidyl methacrylate-Fe3O4 (C18@PS-DVB-GMA-Fe3O4) have been synthesized by using N, N-dimethyloctadecylamine as modifying agent, which could be beneficial to remove the blood phospholipids. The C18@PS-DVB-GMA-Fe3O4 nanoparticles have been used and evaluated in the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) procedure for human plasma prior to the analysis of propofol by supercritical fluid chromatography (SFC). In the QuEChERS procedure, human plasma samples are directly mixed with extraction solvent and C18@PS-DVB-GMA-Fe3O4 nanoparticles, and the extraction and cleanup procedures have been accomplished simultaneously. The SFC separation was performed with a C18 column (Thermo Scientific™ Acclaim™ 120, 250 × 4. 6 mm, 5 μm) within 5 min, using thymol as the internal standard. Supercritical carbon dioxide was used as the mobile phase with methanol as the cosolvent at the flow rate of 1.0 mL/min. The column temperature was 38°C, and detection wavelength was 275 nm. A good linearity was obtained among the propofol concentration range of 0.5-10 mg/L (R2 = 0.9997) with the limit of detection of 0.17 mg/L. Recoveries were in the range of 76.5-91.9%, with RSD less than 7.9%. These results suggested that method is convenient, rapid with high accuracy and little matrix effect, and suitable for rapid determination of propofol plasma concentration.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142466604","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":"Rapid Characterization and Identification of the Chemical Constituents in San-Huang-Xie-Xin-Tang, a Traditional Chinese Medicine Formula, by High Performance Liquid Chromatography Coupled to Electrospray Ionization and Quadrupole Time-of-Flight Mass Spectrometry.","authors":"Lei Liu, Pei Hu, Mengmo Chen, Jiasi Huang, Qing Zhang, Yun Ling","doi":"10.1093/chromsci/bmae056","DOIUrl":"10.1093/chromsci/bmae056","url":null,"abstract":"<p><p>San-Huang-Xie-Xin-Tang (SHXXT), a traditional Chinese medicine formula composed of Coptidis rhizome (CR), Scutellariae radix (SR) and Rhei rhizome (RR), is widely used to treat hypertension, gastritis and peptic ulcer clinically. However, the chemical constituent of SHXXT is still unclear due to its complexity, which hindered the discovery of effective compounds and quality control. Thus, an in-depth understanding of its chemical constituents is very essential. To address this problem, comprehensive analysis of chemical constituents of SHXXT was performed by high performance liquid chromatography coupled to electrospray ionization and quadrupole time-of-flight mass spectrometry (HPLC-ESI-QTOF-MS/MS). As a result, 45 compounds were identified, including 8 phenolic acids, 15 flavonoids, 13 alkaloids, 8 anthraquinones and 1 lignan. Among them, 17 compounds were from CR, 17 compounds were from SR and 11 compounds were from RR. This established method can systematically and rapidly analyze the chemical constituents in SHXXT, which provides chemical foundation for further research on effective substances and action mechanism of SHXXT.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142583067","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":"Stability Indicating RP-HPLC Method by QbD Approach and LC-MS Characterization of Degradation Products of Mifepristone.","authors":"Chandni Chandarana, Isha Juwarwala, Parixit Prajapati, Jaimin Kumar Patel","doi":"10.1093/chromsci/bmaf017","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf017","url":null,"abstract":"<p><p>A Stability indicating revered phase high performance liquid chromatography (RP-HPLC) method have been developed and validated for the estimation of Mifepristone. LC-MS Studies was carried out for identification of possible degradation products. A simple, rapid, accurate and precise stability indicating RP-HPLC method was developed for quantification of Mifepristone. The developed method used the mixture of methanol and water (88:12 v/v) as mobile phase at flow rate of 1 ml /min, which was optimized with the help of Quality by Design approach. Detection was carried out at 305 mm. The linearity of the proposed method was found in the concentration range of 5-25 μg/ml with regression coefficient (R2) of 0.996. LOD and LOQ were found to be 0.0324 and 0.0982 μg/ml, respectively. The recovery of the proposed method was found to be 98%-100%. The method was found to be precise and robust. The developed stability indicating RP-HPLC method was successfully applied for quantification of Mifepristone in pharmaceutical dosage form. The degradation products were characterized by LC-MS and the fragmentation pathways were proposed.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143753008","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 Universal Quantitative Residual Solvent Analysis of Solids and Liquids Using a Full Evaporative Technique and Methanized Flame Ionization Detection.","authors":"Allison Ferranti, Taylor Hayward","doi":"10.1093/chromsci/bmaf014","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf014","url":null,"abstract":"<p><p>Residual solvent analysis is a common method used in the manufacturing of finished goods and pharmaceuticals to ensure the safety of the final product to the consumer. Typically, this involves a headspace sample introduction set up and then separation by gas chromatography (GC) with detection by a flame ionization detector (FID). This analysis can be very time consuming in sample preparation, calibration and analysis time. A full evaporative technique has been applied to both solid and liquid samples for the rapid vaporization of the solvent analytes, which is then introduced to a GC for separation. Additionally, a methanizer was used in line with the FID creating a uniform response for solvents of various heteroatoms and functionalities. This combination of full evaporative technique with a methanized-FID allows for the use of a single response factor for residual solvent analysis with demonstrated repeatability of ˂4%RSD. Spiked solid sample analysis shows recovery between 95% and 105% of solvents tested at ⁓2 μg of each analyte. Overall, the combination of full evaporative headspace sampling and methanized-FID can be applied to any sample matrix for any solvent used in manufacturing or production, making a universal method for residual solvent analysis.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730251","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}
Vineeta V Khanvilkar, Shruti S Mandle, Prachi R Hande, Bhavin R Daka, Pratik P Jadhav
{"title":"RP-HPLC Method Development and Validation for Simultaneous Estimation of Berberine and Ursolic Acid in Formulation.","authors":"Vineeta V Khanvilkar, Shruti S Mandle, Prachi R Hande, Bhavin R Daka, Pratik P Jadhav","doi":"10.1093/chromsci/bmaf016","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf016","url":null,"abstract":"<p><p>Medicines used in ayurveda are typically made of many herbs or are polyherbals. Standardization of these medicines can be carried out by quantitative estimation of two or more of its markers simultaneously. Berberine and ursolic acid are two active markers which are present in an Ayurvedic formulation, Giloy Tulsi tablets. In the present research work, the Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the simultaneous quantitative determination of berberine and ursolic acid from the formulation. With an RP Hemochrom C18 column, chromatographic separation was accomplished at 292 nm with eluent composed of methanol: acetonitrile (4:1, v/v) at a flow rate of 1.0 mL/min. The retention time of berberine and ursolic acid was obtained to be 1.5 ± 0.02 and 3.2 ± 0.02 min, respectively. A simple, rapid, accurate, specific, and robust analytical method was developed to estimate berberine and ursolic acid. This validated method can be used for routine quality control of ayurvedic formulations or herbal formulations having plants which contain berberine and ursolic acid.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730255","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 of Chiral Stationary Phase Based on 1,1'-bi-2-Naphthol for Chiral Enantiomer Separation.","authors":"Kun Fan, Rui Dong, Wenqing Hou, Canyu Yang, Kongchun Sun, LvJing Xu, Bingquan Chang, Desheng Wang, Congcong Zhang, Baochun Shen","doi":"10.1093/chromsci/bmae051","DOIUrl":"10.1093/chromsci/bmae051","url":null,"abstract":"<p><p>Two enantiomeric novel chiral stationary phases (CSPs) R-3-Amide-BINOL CSP (CSP-1) and S-3-Amide-BINOL CSP (CSP-2) were prepared using (R/S)-1,1'-bi-2-naphthol (BINOL) derivatives as chiral selectors. The structure of CSPs was characterized by nuclear magnetic resonance, scanning electron microscope and elemental analysis. Four chiral solutes were selected under normal phase HPLC conditions to evaluate the chiral separation ability of the two novel CSPs. The effects of mobile phase and acidic additives on enantiomeric separation were investigated. The combination of molecular docking simulation and experimental data has elucidated the crucial role of hydrogen bonds and π-π interactions formed between the analyte and CSP in chiral recognition, and different configurations of CSP can cause enantiomeric elution sequence reversal, indicating that the configuration of chiral selectors in CSP has a significant impact on chiral recognition ability.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142347578","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}