{"title":"Rapid and validated LC-APCI-MS/MS method for determination of N-nitroso vonoprazan in pharmaceutical products.","authors":"Filiz Demir, Sıdıka Ertürk Toker","doi":"10.1093/chromsci/bmag024","DOIUrl":"https://doi.org/10.1093/chromsci/bmag024","url":null,"abstract":"<p><p>The primary objective of this study was to develop and validate a liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometric (LC-APCI-MS/MS) method for the determination of trace levels of N-nitroso vonoprazan (NVNP) in vonoprazan active pharmaceutical ingredient (API) and pharmaceutical products. Chromatographic separation was achieved on an Acquity® Premier HSS T3 column under isocratic conditions using 0.1% formic acid in water and acetonitrile as the mobile phase. Detection was performed in positive ion mode using multiple reaction monitoring. The method was validated according to ICH Q2(R2) guidelines for selectivity, linearity, accuracy, precision, robustness, matrix effect, limit of detection (LOD), and limit of quantification (LOQ). The method was linear over the concentration range of 0.24-50.0 ng/mL (R2 = 0.9971), with recoveries of 85.6%-99.2% and relative standard deviation values below 6.1%. The validated LOD and LOQ were 0.10 and 0.24 ng/mL, respectively; the latter corresponds to 0.24 μg/g (240 ppb) in the pharmaceutical product. Matrix effect evaluation showed 91.6% response (8.4% ion suppression), indicating minimal matrix interference. The validated LC-APCI-MS/MS method was successfully applied to both API and finished products and is suitable for routine quality control, stability studies, nitrosamine risk assessment, and regulatory monitoring of NVNP.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148864966","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":"QbD consideration for developing and validating the dissolution test method for quantitative analysis of tadalafil chewable tablets.","authors":"Seung-Hyun Park, Joo-Eun Kim","doi":"10.1093/chromsci/bmag025","DOIUrl":"https://doi.org/10.1093/chromsci/bmag025","url":null,"abstract":"<p><p>Erectile dysfunction (ED) is defined as the persistent inability to achieve or maintain an erection sufficient for satisfactory performance for a duration of >3 months. However, chewable tadalafil formulations for treating ED and corresponding dissolution analysis methods for their quantification are lacking. Therefore, this study aims to investigate Quality by Design considerations for developing a reversed-phase high-performance liquid chromatography method. The test method was designed to perform a quantitative dissolution analysis of tadalafil chewable tablets to enhance medication compliance. This method required an Agilent C8 column (4.6 × 5.0 cm, 5 μm) as the stationary phase and a mobile phase comprising a 1:1 methanol-water mixture. The column temperature and detection wavelength were maintained at 40°C and 225 nm, respectively. The development and validation of the dissolution method resulted in a relative standard deviation of 0.03% for system suitability, assessed in a test solution containing a solubilizer. The test method demonstrated specificity by clearly distinguishing the active pharmaceutical ingredient from excipients. Tadalafil accuracy was confirmed with an average recovery rate of 100.22%, and the precision showed a relative standard deviation of 0.35%. Excellent linearity (R2 = 1.000) was observed over the concentration range of 1.5 μg/mL to 9.0 μg/mL. Additionally, the detection and quantification limits for tadalafil were 0.003 μg/mL and 0.008 μg/mL, respectively. The developed method facilitated rapid quantification of tadalafil in chewable tablets, completing each run within 5 min and reducing analysis time by ~60% compared to conventional methods. Additionally, reagent consumption and operational costs were reduced by ~45%, improving overall efficiency. These findings validate the suitability of the method for reliable industrial quality control of tadalafil chewable tablets and new formulations.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"64 8","pages":""},"PeriodicalIF":1.8,"publicationDate":"2026-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148891741","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}
Sathish Kumar Konidala, Srikar Grandhi, Harsha Sri Kamma
{"title":"Development of a stability-indicating RP-UPLC method for simultaneous determination of Abemaciclib and Olaparib with LC-MS characterization of degradation products and in vitro performance evaluation.","authors":"Sathish Kumar Konidala, Srikar Grandhi, Harsha Sri Kamma","doi":"10.1093/chromsci/bmag022","DOIUrl":"https://doi.org/10.1093/chromsci/bmag022","url":null,"abstract":"<p><p>The simultaneous determination of Abemaciclib and Olaparib in in-houseprepared tablets was accomplished by the development and validation of a novel and rapid and sensitive reverse-phase ultra-performance liquid chromatography (RP-UPLC) technique. Using a Waters X-Bridge C18 (4.6 × 100 mm, 3.5 μm) column and a mobile phase made up of 0.1% orthophosphoric acid in water, acetonitrile and methanol (70:20:10% v/v/v) in an isocratic elution mode at a flow rate of 1 mL/min, the chromatographic separation was accomplished. High sensitivity and selectivity were made possible by performing the detection at 219 nm. Following ICH Q2(R1) criteria, the technique was validated and showed high linearity (R2 > 0.999) for both drugs over the concentration range of 10-60 μg/mL. Within acceptable boundaries (<2% Relative Standard deviation (RSD)), both intra-day and inter-day precision and accuracy (recovery percentage) were proven. Forced degradation studies confirmed the method's stability-indicating capability, Stability studies indicated significant degradation under acid, alkali, peroxide and thermal degradation conditions. The degradation products were characterized by LC-MS technique, and possible degradation pathways were proposed. Additionally, in vitro pharmacokinetic evaluation, including dissolution and drug release kinetics, was performed to assess formulation performance. The developed method proved simple, precise and robust, making it suitable for routine quality control, stability study and pharmacokinetic studies of Abemaciclib and Olaparib co-formulated tablets.</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":"148578731","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":"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}