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":"<p><p>Plasticizers such as phthalate acid esters including di-(2-ethylhexyl) phthalate (DEHP) and its alternatives are commonly found in extractables and leachables (E&Ls) from plastic-based medical devices. Regulatory agencies require manufacturers to monitor, qualify and quantify the E&Ls from medical devices to ensure the safety. Analyzing E&Ls from medical devices is difficult due to the unpredictability and complexity of matrices. The advent of the novel Polyarc/Flame Ionization Detector (FID), which features compound-independent response, provides the opportunity of quantitation of unknowns-to-be-identified E&Ls without using pure substances for establishing calibration. The present work evaluated firstly the feasibility and efficacy of full scan GC-MS with parallel Polyarc/FID system through analysis of plasticizers in E&Ls. In the same injection, E&Ls were identified by full scan GC-MS, then quantified through Polyarc/FID response factor of internal standards. The results showed that quantitation via response factor from internal standards are more accurate so the need for standards of the identified E&Ls is eliminated. The method can combine screening process and target analysis into a one-step execution, which makes it desirable for E&L analysis. The method was applied to a polyvinyl chloride medical device, yielding 1.183 g/device of acetyl tri-n-butyl citrate, 370.2 mg/device of trioctyltrimellitate, and 3.068 mg/device of DEHP.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144325895","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"AQbD-Based Development and Validation of HPTLC Method for Simultaneous Determination of Glycopyrronium, Formoterol Fumarate and Budesonide in Rotacaps.","authors":"Dharati R Saradhara, Vijaykumar K Parmar","doi":"10.1093/chromsci/bmaf033","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf033","url":null,"abstract":"<p><p>Analytical quality by design was used to develop and validate a sensitive, accurate and precise high performance thin layer chromatography method for the determination of glycopyrronium (GLY), formoterol fumarate (FFD) and budesonide (BUD) in pharmaceutical dosage form (Rota caps). Design of Experiment was carried out by Placket-Burman screening design and Box- Behnken response surface methodology using peak area and Rf value as critical method attributes. Method operable design region was navigated for optimization and development of the method. The developed method was validated as per ICH Q2 guidelines. Linearity was found to be 0.25-1.25 μg/band, 0.12-0.60 μg/band and 4-20 μg/band respectively for GLY, FFD and BUD. Accuracy of the method was determined by recovery studies where the percentage recoveries were found to be 98-101%. The precision of the method was determined by repeatability and intermediate precision studies. The % RSD values were found to be less than 2, proving method was precise. The method was found specific and precise for the estimation of drugs. The developed method was applied for the assay of rotacaps and results were found in good agreement with the label claim.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144317008","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jianing Li, Ping Li, Hao Sun, Fan He, Qi Wu, Zhaofang Liu, Shuhong Ye, Yan Ding
{"title":"Quantitative Analysis of Ginkgo biloba Extracts Using a New HPLC Method: Single Standard for the Determination of Multiple Components.","authors":"Jianing Li, Ping Li, Hao Sun, Fan He, Qi Wu, Zhaofang Liu, Shuhong Ye, Yan Ding","doi":"10.1093/chromsci/bmaf032","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf032","url":null,"abstract":"<p><p>In this study, a quality control method utilizing high-performance liquid chromatography has been developed to simultaneously determine the content of 12 major flavonoids in Ginkgo biloba leaf (GBL) through fingerprint analysis and a single standard for the determination of multiple components (SSDMC). Thirteen batches of GBL samples and standardized extracts were analyzed using the SSDMC, traditional external standard (ES) and Chinese pharmacopoeia (CP) methods. The new quality control method was credible and feasible, having been sufficiently validated for linearity (r2 > 0.9993), limits of detection (0.13-0.83 μg/mL), limits of quantification (0.43-2.76 μg/mL), precision (relative standard deviation [RSD] < 0.89%), accuracy (92-114%, RSD < 1.76%), repeatability (RSD < 1.92%) and stability (RSD < 1.96%). The flavone contents observed in the 13 batches of GBL samples and standardized extracts showed no significant difference when using SSDMC and ES methods, and their contents were slightly higher than those obtained using the CP method.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 6","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144266361","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Priya Dubey, Maninder K Vasisht, Subash C Mandal, Jai Malik
{"title":"Design and Optimization of the Extraction Process for Eclipta alba Linn. Using Response Surface Methodology.","authors":"Priya Dubey, Maninder K Vasisht, Subash C Mandal, Jai Malik","doi":"10.1093/chromsci/bmaf025","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf025","url":null,"abstract":"<p><p>Eclipta alba (Family-Asteraceae) is a commercially important plant whose extract is used in numerous marketed formulations as one of the major ingredients. Most of the industries use conventional extraction techniques without considering the marker content extracted. Therefore, the present study was planned to optimize the extraction process for E. alba Linn. using response surface methodology. The powdered plant material was extracted by Soxhlet, reflux, maceration and ultrasonication using four solvents namely acetone, ethanol, 50% aqueous ethanol and 80% aqueous ethanol for each technique. Particle size, powder-to-solvent ratio and duration of extraction were other three variables used to optimize the extraction procedure. The extraction procedure was optimized on the basis of the weight of the extract and wedelolactone (the main bioactive marker) content using the response surface methodology with the Box-Behnken design. Soxhlet extraction using 50% aqueous ethanol with extraction time (4.65 h), powder-to-solvent ratio (5.29%w/v) and particle size (1.19 mm) gave best extract yield (900.04 mg) and wedelolactone content (0.4161%). The results showed that the proposed methodology can help in obtaining the maximum extraction yield thereby improving the quality and reproducibility of extract of this commercially important plant, and will also help in reducing production time and cost.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144020072","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}
Mohamed Abouzid, Julia Kerner, Aniceta Mikulska-Sauermann, Dorota Filipowicz, Matylda Resztak, Franciszek Główka, Leonid Kagan, Marta Karaźniewicz-Łada
{"title":"Extension of an Ultra-High Performance Liquid Chromatography-MS/MS Method for the Determination of C3 Epimers of 25-Hydroxyl Derivatives of Vitamin D in Human Plasma.","authors":"Mohamed Abouzid, Julia Kerner, Aniceta Mikulska-Sauermann, Dorota Filipowicz, Matylda Resztak, Franciszek Główka, Leonid Kagan, Marta Karaźniewicz-Łada","doi":"10.1093/chromsci/bmaf031","DOIUrl":"10.1093/chromsci/bmaf031","url":null,"abstract":"<p><p>Current vitamin D quantification methods do not account for 25-hydroxyl epimers, which can falsely increase concentrations and mask actual deficiencies. Previously, we developed an ultra-high performance liquid chromatography-tandem mass spectrometry method to measure 25(OH)D3, 3-epi-25(OH)D3 and 25(OH)D2; here, we extended this method to include 3-epi-25(OH)D2. Analytes were separated using a Shimadzu UPLC with a Kinetex F5 column (100 × 2.1 mm, 2.6 μm). The mobile phase contained 0.1% formic acid in methanol and water (70:30, v/v). The internal standard, deuterated 25(OH)D3 and analytes were extracted with hexane. Detection was performed by a mass spectrometer equipped with a triple quadrupole after prior electrospray ionization. It demonstrated sufficient precision and spike recovery within and between days, with a coefficient of variation ≤15% and an error of determination ≤18%. The method exhibited linearity in the 2-100-ng/mL concentration range. The limits of quantification and limits of detection were 2 and 1 ng/mL, respectively. Extraction recoveries ranged from 70.05% to 97.13%. The matrix effect, carryover and dilution integrity were evaluated and met the FDA acceptance criteria. The stability of all metabolites in plasma was confirmed after 3 h of storage at room temperature and after three cycles of freezing at -80°C and thawing. Applying the method to clinical samples showed a high 25-hydroxyl epimer derived from vitamin D.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12123413/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144187140","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":"Magnetic Carbon as an Adsorbent for the Enrichment of Carbamate Pesticides in Magnetic Solid Phase Extraction Prior to High Performance Liquid Chromatography.","authors":"Poonsiri Homchun, Jirasak Gamonchuang, Rodjana Burakham","doi":"10.1093/chromsci/bmaf030","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf030","url":null,"abstract":"<p><p>A simple one-step synthesis method was proposed to prepare magnetic carbon material, which were subsequently employed for the magnetic solid phase extraction of carbamate pesticides prior to their determination by high performance liquid chromatography. The optimized condition resulted in the efficient extraction of a 30-mL sample solution using 50 mg of magnetic carbon as a sorbent, a 2-min vortex loading time and 1000 μL of acetone as an elution solvent with a 3-min vortex elution. The linear range of the proposed method was 5-200 μg L-1, with limits of detection and quantitation in the ranges of 3-40 and 5-60 μg L-1, respectively. The relative standard deviations were <9.5%, which indicated a high level of precision. The results suggested that the proposed magnetic solid phase extraction method was an effective enrichment procedure and could be effectively implemented for the determination of carbamate pesticides in fruit samples. Satisfactory recoveries in the range of 70.2%-120.0% were obtained with the relative standard deviations of <11.6%. The method provided the benefit of a rapid extraction process, and the magnetic carbon functioned as an eco-friendly adsorbent that could be prepared in an easy manner.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144187141","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 Determination of 30 Flavonoids in Jinqiancao Granules by LC-MS/MS.","authors":"Jiajie Wang, Yimeng Liu, Shuang Xie, Luyao Wang, Beibei Yao, Xu Zhang, Wanwan Zhang, Chunying Wang","doi":"10.1093/chromsci/bmaf028","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf028","url":null,"abstract":"<p><p>In order to determine the content of flavonoid components in Jinqiancao granules efficiently and accurately, a high-efficiency quantitative analysis method utilizing liquid chromatography-tandem mass spectrometry (LC-MS/MS) was employed. As per the guidelines from the International Council for Harmonization, a comprehensive method validation was conducted for this method. Experimental data demonstrated that the method exhibited excellent accuracy, specificity and reproducibility in the multiple reaction monitoring mode, facilitating the swift and accurate quantification of flavonoid content. Through chemometrics analysis, significant differences in the content of flavonoid compounds were observed among different batches of Jinqiancao granules samples. Isoschaftoside, Vicenin-2, Schaftoside and myricitrin can be used as the main quality markers for Jinqiancao granules. The research results provided a scientific basis for the quality control of Jinqiancao granules, which helps enhance the consistency and reliability of the product, thereby ensuring the superior quality of the preparation.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144111062","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}
Geovanna Soldi, Bernardo Augusto de Freitas Dornelas, Mario Ferreira Conceição Santos, Giulia Stavrakas Miranda, Geraldo Humberto Silva
{"title":"Development of a solid phase extraction-high-performance liquid chromatography-ultraviolet detector method for quality control of the rosemary-pepper tincture, a phytotherapic produced by living pharmacies in Brazil.","authors":"Geovanna Soldi, Bernardo Augusto de Freitas Dornelas, Mario Ferreira Conceição Santos, Giulia Stavrakas Miranda, Geraldo Humberto Silva","doi":"10.1093/chromsci/bmaf027","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf027","url":null,"abstract":"<p><p>Ensuring the accurate measurement of the active components in herbal medicine is critical in maintaining their clinical effectiveness. One quality-controlled medicine is the rosemary-pepper tincture, a hydroalcoholic extract of Lippia sidoides leaves that contains the active ingredient, thymol. It is used as an antiseptic to treat injuries. Thus, a validated method for standardizing the active component was developed to extract the thymol and eliminate polar and nonpolar interferents, thereby extending the lifespan of the chromatographic column. To evaluate the adsorption of thymol into the flow, the adsorption data were adjusted using the Thomas model to obtain the maximum amount of adsorption, 4.33 mg/g. Factorial planning revealed that the best conditions for the adsorption and desorption of thymol were 1.4 mL of tincture in an SPE-C18 column and 2 ml of methanol/water (80/20) as eluent. Subsequently, the thymol was quantified using HPLC-UV spectroscopy, and the calibration curves were linear in the working range of 0.1-1.0 mg/mL (R2 = 0.997). The limits of detection and quantification were 0.02 and 0.06 mg/mL, respectively. The precision and accuracy were 95.8-103.8% at three different concentrations. Finally, the method proved robust against multiple applied variations and yielded satisfactory results within the analysis parameters.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144159366","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":"Determination of Fungicides in Fresh Fruit Juice Using Magnetic Solid-Phase Extraction Coupled With Gas Chromatography-Triple Quadrupole Mass Spectrometry.","authors":"Qinghua Yang, Honghai Deng, Yilan Shi, Qianying Qiu, Jinxin Wang, Wenhui Ping, Jun Gu, Weibing Zhang","doi":"10.1093/chromsci/bmaf024","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf024","url":null,"abstract":"<p><p>A fast, simple and effective method was developed and validated for determination of 11 fungicides using magnetic solid-phase extraction with NH2-Fe3O4@GO (graphene oxide) combined with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). To carry out the extraction of the fungicides from samples, NH2-Fe3O4@GO nanocomposites were synthesized and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The target analytes were extracted on NH2-Fe3O4@GO and then eluted by ethyl acetate and acetonitrile (1:1 v/v). Finally, the extraction solvent concentrated by nitrogen blowing was analyzed by GC-MS/MS, which demonstrated good linearity between 0.05 and 5.0 mg L-1. The limits of detection (signal-to-noise ratio = 3) and the limits of quantification (signal-to-noise ratio = 10) for the 11 fungicides ranged from 1.0 to 3.5 and 3.0 to 10.5 μg kg-1, respectively. The accuracy and precision of the proposed method were evaluated by measuring tagged samples; the recoveries and relative standard deviations ranged from 75.3% to 103.9% and 2.19% to 4.68%, respectively. The utility of the adsorbent was demonstrated to determine trace fungicides in fresh fruit juice samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144002756","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 Assay Method and LC-MS Characterization of Forced Degradation Products of Pantoprazole and Aspirin.","authors":"Tinkal S Patel, Ankit B Chaudhary","doi":"10.1093/chromsci/bmaf029","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf029","url":null,"abstract":"<p><p>To assess the degradation of the drug under forced degradation, stability experiments with aspirin and pantoprazole were performed. Under the guidelines set forth by the International Conference on Harmonization, pantoprazole and aspirin were exposed to oxidation, alkaline and acidic hydrolysis and thermal stress. Under basic and acidic hydrolysis stress, the drug combination demonstrated significant degradation. Under conditions of oxidative stress and heat, however, it remained stable. A mobile phase, containing methanol: ammonium acetate buffer (0.01 M) (70: 30% v/v) was employed, a column (250 mm × 4.6 mm, and 5 μm), detection wavelength was 254 nm, flow rate of 0.8 mL min-1 was used. The degradation products were identified using LC-MS, and fragmentation paths were suggested. (Graphical abstract: Figure 1).</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 5","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144159369","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}