{"title":"Identification and characterization of chemical constituents in Scutellariae barbatae Herba by UHPLC-QTOF-MS.","authors":"Xuelin Zong, Zhang Qin, Zhu Hui, Zhao Ying, Xun Gao, Shi Yun, Kunming Qin","doi":"10.1093/chromsci/bmag023","DOIUrl":"https://doi.org/10.1093/chromsci/bmag023","url":null,"abstract":"<p><p>Scutellariae barbatae Herba, the dried whole plant of S.barbatae D. Don, has been documented in the Chinese Pharmacopoeia since 1985. The chemical constituents of S. barbatae Herba are complex. And comprehensive analysis of the chemical components in S. barbatae Herba is still scarcely studied. In this study, ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was used in both negative and positive ion modes to comprehensively analyze chemical constituents of S. barbatae Herba. Moreover, the fragmentation pathways of compounds were explained in brief. According to tandem mass spectrometry fragmentation data and previous reports, a total of 39 compounds were identified, including 19 flavonoids, 4 neo-clerodane diterpenoids, 1 neo-clerodane diterpenoid alkaloid, 3 triterpenes, 5 fatty acids, 1 lignin, 1 monoterpene phenol, and 4 other constituents. More fragments of information are formed in the compounds, and the fragmentation pathways were explained simply. The developed analytical method is simple, reliable, and effective, providing comprehensive information on the metabolite profile of S. barbatae Herba, which may enhance its quality control and further utilization.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 7","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148793814","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 quantitation of oleanolic and ursolic acids by RP-HPLC-DAD on active ingredient from Tabebuia hypoleuca leaves.","authors":"Luz María Sánchez Perera, Susandy Hernández Méndez, Chouaha Bouzidi, Raphaël Grougnet","doi":"10.1093/chromsci/bmag021","DOIUrl":"https://doi.org/10.1093/chromsci/bmag021","url":null,"abstract":"<p><p>The genus Tabebuia is widely used in traditional medicine of tropical and subtropical countries. We recently reported the antitumor activity toward several human cell lines of the ethyl acetate extract of the leaves of Tabebuia hypoleuca, a species endemic to Cuba, together with the high content of triterpenic acids. This work describes the development and the validation of a reversed-phase high-performance liquid chromatography with diode array detection method for the simultaneous quantitation of the contents of oleanolic acid (OA) and ursolic acid (UA). The method was carried out on a C18 column, using methanol and water as mobile phase (ratio 95:5 v/v), at the flow rate of 0.4 mL/min, recorded at λ = 210 nm. The retention times were 16.371 ± 0.045 and 16.943 ± 0.052 min for OA and UA, respectively, with a resolution between peaks of 1.29. The average contents of OA and UA within three sets of the ethyl acetate extract, considered as an active pharmaceutical ingredient (API) were 102.93 and 244.28 mg/g, respectively. The linearity of the response was found to be 10-700 μg/mL for OA and its equation was y = 0.2946x - 2.0432 (r2 = 0.9924). The linearity range for UA was 5-1000 μg/mL and its equation was y = 0.3284x - 17.508 (r2 = 0.9865). The limit of detection and limit of quantification of these constituents were 6.50 and 19.81 μg/mL for OA, 0.75 and 1.98 μg/mL for UA. OA and UA may be used as markers for the quality assessment of formulations containing this API. The developed method is accurate, specific, precise, reproducible and may be applied as a simple and rapid quality-control procedure for medicinal plant extracts with similar triterpene patterns.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 6","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148277700","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}
Hamzeh Adelpour Abdoli, Kamal Alizadeh, Payman Hashemi
{"title":"A new device for simultaneous cooling of the drop and evaporated sample for the extraction of volatile components using cooled side arm tube headspace microextraction.","authors":"Hamzeh Adelpour Abdoli, Kamal Alizadeh, Payman Hashemi","doi":"10.1093/chromsci/bmag020","DOIUrl":"https://doi.org/10.1093/chromsci/bmag020","url":null,"abstract":"<p><p>A new cooled side arm tube headspace single drop microextraction (CSAT-HS-SDME) method was successfully applied to the extraction of Carum copticum volatile components. The aim of this research is to design and fabricate a new device for simultaneous cooling of the drop and evaporated sample. The innovated technique was evaluated by the extraction and Gas chromatography-mass spectrometer (GC-MS) determination of p-cymene, γ-terpinene and thymol in C. copticum samples. Optimization of the effective extraction parameters was carried out by the simplex method. Under the optimized conditions (i.e. cold and heat temperature, -10°C and 70°C; water addition, 20 μL and extraction time, 20 min), the relative standard deviations of peak areas obtained from five replications were between 3.62% and 4.69%. Compared to other similar equipment for cooling the extraction phase and simultaneously heating the sample, this device has advantages such as simplicity, very low cost, ease of use, portability and no need for additional equipment such as a liquid carbon dioxide cylinder or heater-stirrer. The proposed method was successfully applied to the extraction and identification of volatile components of some C. copticum samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 6","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148338752","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 gas chromatography-mass spectrometry method for identification and quantification of selected non-intentionally added substances IN pharmaceutical formulations.","authors":"Stuti Pandya, Nasir Vadia, Navin Sheth","doi":"10.1093/chromsci/bmag019","DOIUrl":"10.1093/chromsci/bmag019","url":null,"abstract":"<p><p>In recent years, the government of India has banned single-use plastic, as it is more customer-friendly but poses major disadvantages, such as leaching. As impurities can be present in any source, from the raw material to the end product, and so on, these are scientifically termed extractables and leachables. To identify these types of impurities from the pharmaceutical formulation, predominantly parenteral and ophthalmic or any other products available in plastic packaging, a rapid, selective, and simultaneous method for four different analytes has been developed with the help of gas chromatography-mass spectrometry and validated completely according to International Council for Harmonization Q2(R1) guidelines. Selected extractables and leachables, namely cyclohexanone, 2,4,7,9-tetramethyl-5-decyne-4,7-diol, bis(2-ethylhexyl) sulfosuccinate sodium salt, and benzophenone, were detected by mass spectrometry and identified using the NIST17 library of the instrument. The developed method was within the range.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 5","pages":""},"PeriodicalIF":1.3,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148156765","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":"Investigation of surface properties of various parts of Angelica sylvestris by inverse gas chromatography.","authors":"Melek Kubra Habiboglu, Birol Isik, Fatih Cakar","doi":"10.1093/chromsci/bmag017","DOIUrl":"10.1093/chromsci/bmag017","url":null,"abstract":"<p><p>There are nine different varieties of Angelica sylvestris plants found in Asia, America, and Europe, and all of them, especially their roots, have medicinal properties. It is important to determine the surface properties of medicinal A. sylvestris that can be easily found in nature. In this study, it was aimed to investigate the surface characteristics of the root, stem, and flower parts of the A. sylvestris. For this purpose, gas chromatography columns were prepared by separating the root, stem, and flower parts of the plant, and the surface properties were determined by the inverse gas chromatography (IGC) method. The IGC study was performed at infinite dilution with polar and non-polar solvents. Surface characteristics of different parts of the plant were determined through analysis of retention diagrams. From IGC experiments, the changes in the acidic and basic character of the parts of the plant were determined and compared with each other. As a result of this comparison, it was found that all KD/KA values were less than 1 and changed as flower > root > stem.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 5","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13174400/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147941545","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Malavika Thiruvenkatakumar, Hariprasad Ranganathan, Habibur Rahman S M
{"title":"Development and validation of stability-indicating RP-HPLC method for simultaneous estimation of clomiphene citrate and co-enzyme Q10 in bulk and pharmaceutical dose.","authors":"Malavika Thiruvenkatakumar, Hariprasad Ranganathan, Habibur Rahman S M","doi":"10.1093/chromsci/bmag013","DOIUrl":"10.1093/chromsci/bmag013","url":null,"abstract":"<p><p>Clomiphene citrate (CLO) and co-enzyme Q10 (Q10) are \"ovulatory stimulants\" used to treat female infertility and CLO-resistant Polycystic Ovary Syndrome (PCOS). The study aimed to create a unique and well-validated stability-indicating RP-HPLC method for quantifying CLO and Q10 in bulk and tablet formulation, supported by UV analysis. The λ max values of CLO and Q10 were determined at 293 nm and 273 nm, respectively. The chromatographic separation was achieved on a Waters XBridge phenyl 5 μm column (4.6 × 250 mm) using an acetonitrile: tetrahydrofuran (80:20 v/v) with 0.5% triethylamine as a mobile phase at a flow rate of 0.5 mL/min with photodiode array detector at 279 nm (isobestic point). Resveratrol (RES) served as an internal standard (ISTD), with retention durations of 6.504, 9.319 and 5.831 minutes for CLO, Q10 and RES, respectively. Calibration curves were linear (R2 = 0.9987 for CLO and 0.9993 for Q10) and %RSD values for all validation parameters were below 2%, confirming precision and accurate. Forced degradation studies through various stress conditions, assessed the method's stability-indicating nature by exhibiting clear separation of degradation products from the analytes and degradation levels within ICH limits (≤ 20%). The validated method was found to be reliable, specific, and applicable for routine analysis in quality control.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 5","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147815444","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 simple method for the determination of Atrazine in lake water by gas chromatography with electron capture detector (GC-ECD) using dispersive liquid-liquid microextraction (DLLME).","authors":"Angélica de Fátima Bortolato Piccioli, Affonso Celso Gonçalves, Bianca Pierina Carraro, Emanuel Sobocinsk Zanini","doi":"10.1093/chromsci/bmag018","DOIUrl":"https://doi.org/10.1093/chromsci/bmag018","url":null,"abstract":"<p><p>Atrazine (ATZ) is a persistent herbicide found in aquatic environments worldwide, and the evaluation and monitoring of potential contamination by this pesticide are of utmost importance. A properly validated and well-established analytical method is important to detect ATZ in the environment. In this work, a dispersive liquid-liquid microsyringe extraction method was developed for the pre-concentration of ATZ in lake water samples for subsequent determination in a gas chromatograph with an electron capture detection (GC-ECD) system. The method showed excellent linearity in the range of 2 μg L-1 to 30 μg L-1, with correlation coefficient (R) values ≥0.995. In addition, the method is selective, and the sample matrix does not interfere with the determinations (≤20%). The limits of detection and limits of quantification were 0.6 μg L-1 and 2 μg L-1, respectively. The method is accurate, with recoveries ranging from 100% to 114%, and precise (13%). The extraction method associated with GC-ECD is reliable, sensitive, simple, fast, reproducible, environmentally friendly and economical. The method was applied to water samples from the Municipal Lake of the city of Cascavel (PR, Brazil) and no ATZ was detected in any of the samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 5","pages":""},"PeriodicalIF":1.3,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148042324","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 bioanalytical method development and validation of ibuprofen and phenyramidol HCl in human plasma using high-performance liquid chromatography with photodiode array detection and its application in a pharmacokinetic study.","authors":"Nurgul Kızıltas, Tugrul Cagri Akman, Yasemin Karabayir","doi":"10.1093/chromsci/bmag015","DOIUrl":"10.1093/chromsci/bmag015","url":null,"abstract":"<p><p>The co-administration of ibuprofen (IBU) and phenyramidol HCl (PHE) is frequently preferred for the management of musculoskeletal disorders to enhance therapeutic efficacy. This study aimed to develop and validate a rapid, sensitive and cost-effective high-performance liquid chromatography-photodiode array (HPLC-PDA) method for the simultaneous determination of IBU and PHE in human plasma and pharmaceutical preparations, and to demonstrate its applicability in pharmacokinetic studies. Chromatographic separation was achieved on a C18 column using a mobile phase consisting of phosphate buffer (pH 6.0 ± 0.05) and methanol (30:70, v/v) at a flow rate of 1.0 mL·min -1. The retention times of IBU and PHE were 3.7 and 2.7 min, respectively, with a total analysis time of 6 min. The method showed excellent linearity within the range of 0.05-40.0 μg·mL -1 for both drugs, with LLOQ values of 0.05 μg·mL-1 for IBU and 0.0025 μg·mL-1 for PHE. The plasma samples were collected at four time points (0.0, 1.0, 4.0 and 8.0 h) after oral administration of IBU and PHE. Cmax, Tmax and AUC0-8 were calculated, with Cmax of 16.14 μg·mL-1 for IBU and 3.71 μg·mL-1 for PHE, while Tmax was 1.0 h for both. Despite limitations in the number of sampling time points, the method proved highly applicable for determining pharmacokinetic profiles and for routine quality control analyses. Its short analysis time, high sensitivity and low sample volume requirement make it a powerful tool for clinical research and therapeutic monitoring. This is the first validated HPLC-PDA method applied to the simultaneous pharmacokinetic evaluation of IBU and PHE in human plasma.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 5","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13130206/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147772866","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Greenness Assessment and Quantitative Profiling of Glycyrrhizic Acid, Piperine and Ursolic Acid Content in Polyherbal Cough Syrup Using High-Performance Liquid Chromatographic Analysis.","authors":"Payal Chauhan, Falguni Tandel, Aboli Girme, Lal Hingorani, Rakesh Parmar","doi":"10.1093/chromsci/bmag009","DOIUrl":"10.1093/chromsci/bmag009","url":null,"abstract":"<p><p>The increasing demand for safe, effective and sustainable alternatives to traditional cough suppressants has brought polyherbal formulations in respiratory ailment management. This report outlines the development and greenness evaluation of a high-performance liquid chromatography method for the simultaneous quantification of glycyrrhizic acid, piperine and ursolic acid from crude plant extracts and commercial polyherbal cough syrups. Chromatographic separation was performed using Agilent Eclipse C18 column (250 × 4.6 mm, 5 μm) under gradient elution using 0.1% formic acid in water and acetonitrile as mobile phases. The optimal absorbance wavelengths during quantification were 254 nm for glycyrrhizic acid, 342 nm for piperine, and 210 nm for ursolic acid at retention times of 21.3, 24.5 and 31.0 min, respectively. Results indicated a method that was sensitive, reproducible and specific to the three analytes quantified as well as validated according to ICH Q2(R1). Evaluating the greenness of the method (using the Analytical GREEnness metric, Green Analytical Procedure Index, and Eco-Scale Assessment confirmed that this method could be considered \"green\". Upon completion of method validation, the method was used to quantify each marker compound from commercially available products in an effort to better understand production methodologies and directed our quality control and standardization efforts. The results of this systematic investigation point to the advantage of applying green analytical techniques for the assessments of polyherbal medicines, potentially establishing them as credible, environmentally friendly therapeutic options for respiratory ailments.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 4","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147592445","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 Reverse-Phase High-Performance Liquid Chromatography Method for Simultaneous Quantification of Tofacitinib Citrate and Berberine Chloride in Bulk, Injection and Plasma.","authors":"Monika, Vikas Jhawat, Mahima Chauhan, Samrat Chauhan, Sonali, Mayank Kumar Singh, Rahul Singh, Rahul Pratap Singh","doi":"10.1093/chromsci/bmag010","DOIUrl":"10.1093/chromsci/bmag010","url":null,"abstract":"<p><p>The main aim of this study was to develop and validate a new reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of tofacitinib citrate (TFC) and berberine chloride (BBC) in pharmaceutical injection formulations and blood plasma. An isocratic RP-HPLC method was used with a mobile phase consisting of phosphate buffer saline (pH 5.5) and acetonitrile at a ratio of 70:30, at flow rate of 1 mL/min at 25°C. Both drugs were detected at 306 nm. The proposed method demonstrated excellent linearity over a concentration range of 5-30 μg/mL for both the TFC and BBC, with correlation coefficients (R2) exceeding 0.999. System suitability parameters, including peak area, tailing factor, theoretical plates and resolution, were within acceptable limits, with relative standard deviations <2%. The recovery studies at 50, 100 and 150% showed mean recovery rates of 99.4-100.7% for TFC and 99.9-100.4% for BBC. The method exhibited high sensitivity, with low detection and quantification limits. The robustness was confirmed under slight variations in flow rate and mobile phase composition. The developed RP-HPLC method is accurate, reliable and suitable for simultaneous quantification of TFC and BBC in pharmaceutical and biological matrices, offering potential for routine quality control and pharmacokinetic studies.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 4","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147592475","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}