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}
{"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}
Mehdi Ashraf-Khorassani, William M Coleman Iii, Tripp Aardema
{"title":"High-Performance Liquid Chromatography Using Ultraviolet Detection for Separation of Terephthalic Acid and Associated Impurities from Recycled Materials.","authors":"Mehdi Ashraf-Khorassani, William M Coleman Iii, Tripp Aardema","doi":"10.1093/chromsci/bmaf026","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf026","url":null,"abstract":"<p><p>An optimized rapid and precise high-performance liquid chromatography method has been developed to separate, identify and quantitate impurities contained within terephthalic acid (TPA) produced from recycled materials. Using a Waters X-Select HSS T3 column for the separation of recycled TPA and eight impurities, and a mobile phase of H2O/CH3CN containing 0.1% trifluoroacetic acid (TFA) with detection by UV at 250 nm, baseline separation of all compounds was achieved in ˂17 min. Four different mobile phase acidic additives were tested, the results indicating that mobile phases with lower pH provided better separation of the compounds with accompanying improved peak shapes. Among all the acidic additives tested in this study, a mobile phase containing 0.1% TFA demonstrated the highest resolution and the best peak shapes. It was concluded that by suppressing the ionization of the acidic compounds contained in the samples through increased acidity of the mobile phase, better peak shapes and higher resolution could be achieved. The amount of increased mobile phase acidity was based in part on the pKa values of the analytes and adjusted so as to eliminate as much as possible any dissociation of the organic acids. A comparison of a standard addition method versus an external calibration curve approach for the quantification of impurities showed similar results, even for relatively low-concentration analytes at levels below 10 ppm. The aspects often linked with validated analytical methods were addressed including linearity, limit of detection, limit of quantitation, sensitivity and selectivity, addressing the criteria set forth in the acronyms of the QuECHERS method description, that is quick easy, cheap, effective, rugged and safe.</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":"144009468","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}
Simonetta Gemma, Giuseppina Multari, Francesca R Gallo
{"title":"An High Performance Thin Layer Chromatography (HPTLC) Validated Method for the Determination of Ephedrine Alkaloids in Multi-Plant Formulations.","authors":"Simonetta Gemma, Giuseppina Multari, Francesca R Gallo","doi":"10.1093/chromsci/bmaf020","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf020","url":null,"abstract":"<p><p>Ephedrine is one component of a popular traditional Chinese multi-plant formulation used to treat asthma, fever, coughs and lately COVID-19. The aim of this study is to develop and validate a simple and rapid quali-quantitative High Performance Thin Layer Chromatography (HPTLC) densitometry method to detect ephedrine, the most abundant alkaloid of Ephedra plant, and to analyze free sale ephedra-based capsules. This quick, simple and low requirement method is cost-effective and allows screening up to 19 samples all together in a single layer. During the development of this method, an extraction solvent mixture composed of methanol/water (2:1, v/v) and a mobile phase constituted of ammonia/methanol/dichloromethane (1:10:40, v/v/v) gave the best results. The identity and purity of ephedrine peak were confirmed by matching Rf value and UV-spectrum with its reference standard. Lastly, samples were quantitated by densitometry at 500 nm after ninhydrin derivatization. Linearity was obtained in the concentration range of 0.062-0.146 μg/band. Limit of detection and limit of quantification (LOQ) were found to be 0.0020 μg/band and 0.0067 μg/band, respectively. This technique is useful to screen multiple samples at the same time with a limited use of solvents and reagents so that it can be considered a fast and simple procedure.</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":"143987871","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":"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}
Wei Wang, Tiebing Liu, Qingyan Li, Enhui Ji, Weizhe Xu, Shi Qiao, Yujing Cui, Boye Li, Haishan Xu
{"title":"Validation of a Sensitive, Simple and High-Throughput UPLC-MS/MS Method for Quantification of Catecholamines and Their Metabolites in Serum and Urine: Application in Clinical Analysis.","authors":"Wei Wang, Tiebing Liu, Qingyan Li, Enhui Ji, Weizhe Xu, Shi Qiao, Yujing Cui, Boye Li, Haishan Xu","doi":"10.1093/chromsci/bmaf021","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf021","url":null,"abstract":"<p><p>A sensitive, simple and high-throughput UPLC-MS/MS method has been validated for the simultaneous quantification of catecholamines and their metabolite levels in serum and urine for clinical applications. The analytes and their isotope-labeled internal standards were extracted using a 96-well solid-phase extraction cartridge and then separated on an HSS PFP column with a 4-min gradient elution. The linear ranges were 10 ~ 5000 pg/mL for dopamine (DA), epinephrine (E), metanephrine (MN) and normetanephrine (NMN), 2 ~ 5000 pg/mL for norepinephrine (NE), and 2 ~ 2000 pg/mL for 3-methoxytyramine (3-MT). The limits of quantification were 10 pg/mL for DA and E, 5 pg/mL for MN and NMN, 2 pg/mL for 3-MT, and 20 pg/mL for NE. The accuracy was excellent with relative bias all within 10%, and the intra-day and inter-day precision values were also within the tolerance range (RSD < 15%), and the recovery was in the range of 86.0-107.7% with RSD < 15%. After correction using IS, no significant matrix effects were observed. Moreover, the discrepancies in the analyte levels between plasma and serum were investigated for the first time. The analyte levels in the two biological matrices exhibited a significant correlation (P < 0.001) and significant differences (P < 0.001).</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":"144002641","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":"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}