Journal of chromatographic science最新文献_第2页

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. 灵敏、简便、高通量UPLC-MS/MS测定血清和尿液中儿茶酚胺及其代谢物的方法验证：在临床分析中的应用

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf021

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":"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).","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}

引用次数: 0

Stability Indicating High Performance Liquid Chromatography Method Development, Validation, and Characterization of Forced Degradant Product by Liquid Chromatography-Mass Spectroscopy for Molnupiravir and Favipiravir. 莫那匹拉韦和法匹拉韦强制降解产物的液相色谱-质谱联用方法的开发、验证和表征。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf015

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":"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.","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}

引用次数: 0

Development and Validation of Rapid and Cost-Effective RP-HPLC/UV Method for Determination of Cetirizine/Levocetirizine in Blood Plasma of Smokers and Non Smokers: a Two Cohort Comparative Study. 用于检测吸烟者和非吸烟者血浆中西替利津/左西替利津含量的快速、经济高效的 RP-HPLC/UV 方法的开发与验证：一项双队列比较研究。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmae058

Mashal Khattak, Zafar Iqbal, Asif Jan, Niaz Ali, Fazli Nasir, Naila Shahbaz

{"title":"Development and Validation of Rapid and Cost-Effective RP-HPLC/UV Method for Determination of Cetirizine/Levocetirizine in Blood Plasma of Smokers and Non Smokers: a Two Cohort Comparative Study.","authors":"Mashal Khattak, Zafar Iqbal, Asif Jan, Niaz Ali, Fazli Nasir, Naila Shahbaz","doi":"10.1093/chromsci/bmae058","DOIUrl":"10.1093/chromsci/bmae058","url":null,"abstract":"In this research study, a simple, rapid, sensitive, and cost-effective Reverse Phase High Performance Liquid Chromatography method was developed and validated for determination of Cetirizine and Levocetirizine in human plasma. The drugs were separated on an ACE Generix100-5 C18 RP (250 × 4.6 mm, 5 μm) column, using Acetonitrile and Distilled water pH 7 (59:41 v/v) as mobile phase with a flow rate of 1.5 mL/min, retention time of 3.39 ± 0.02 min, detection wavelength of 230 nm, and column oven temperature at 26°C. The drug was extracted from human plasma using Methanol, the percent recovery was 97%. The LOD and LOQ for Cetirizine and Levocetirizine were 0.5 ng and 1 ng. The method was linear over the concentration range of 0.5-1000 ng /mL for Cetirizine and Levocetirizine. The method was applied for analysis of drugs in plasma following oral administration of Cetirizine (10 mg) and Levocetirizine (5 mg) in smokers and nonsmokers of Pashtun ethnicity belonging from different districts of Khyber Pakhtunkhwa, Pakistan. The difference between Cetirizine plasma levels in smokers and non-smokers was significant with p -value 0.0279.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142621373","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Novel Green Chromatographic Approaches for Estimation of a Triple Common Cold Pharmaceutical Combination. 估算常见感冒药三联复方的新型绿色色谱法

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmae050

Rabab M Soliman, Yasmin Rostom, Yasmin M Fayez, Nadia M Mostafa, Hany H Monir

{"title":"Novel Green Chromatographic Approaches for Estimation of a Triple Common Cold Pharmaceutical Combination.","authors":"Rabab M Soliman, Yasmin Rostom, Yasmin M Fayez, Nadia M Mostafa, Hany H Monir","doi":"10.1093/chromsci/bmae050","DOIUrl":"10.1093/chromsci/bmae050","url":null,"abstract":"Nowadays, there is a strong interest in the scientific community in developing innovative methodologies within a green analytical chemistry framework. Herein, we introduce the first chromatographic approaches for the concurrent estimation of paracetamol (PAR), carbinoxamine (CRX), and pseudoephedrine (PSE) intended to relieve COVID-19 and common cold symptoms. The first method was thin layer chromatography (TLC) densitometry, which depends on the separation of the studied medications on TLC silica gel plates using ethyl acetate: methanol: ammonia (7.0: 3.0: 0.2, by volume) as the developing system, and were scanned at 208.0 nm. The data were linear in the ranges of 1-25 μg/band for PAR, 1-25 μg/band for PSE and 0.1-5 μg/band for CRX. The second method was reversed-phase high-performance liquid chromatography separation on a Kromasil C18 column using a mixture of 0.01 M phosphate buffer containing 0.1% triethylamine (pH 3.5) adjusted with orthophosphoric acid and ethanol at a flow rate of 1.0 mL/min in a gradient program. The separated peaks were detected at 215.0 nm over a concentration range of 10-250 μg/mL for PAR, 5-35 μg/mL for PSE, and 0.5-25 μg/mL for CRX. Both approaches were validated according to International Conference on Harmonization (ICH) guidelines. Finally, the impact of these methods on the environment was evaluated by many tools.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142347577","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Qualitative, Quantitative Analysis and Pharmacokinetic Study of Potentially Active Components of Huangxueyishen Decoction Based on UPLC-MS/MS. 基于UPLC-MS/MS的黄血益肾汤潜在有效成分定性、定量分析及药动学研究

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf022

Xiaojing Qian, Ying Chen, Song Wang, Jian Chen, He Wang, Cheng Hu, Shan Lin

{"title":"Qualitative, Quantitative Analysis and Pharmacokinetic Study of Potentially Active Components of Huangxueyishen Decoction Based on UPLC-MS/MS.","authors":"Xiaojing Qian, Ying Chen, Song Wang, Jian Chen, He Wang, Cheng Hu, Shan Lin","doi":"10.1093/chromsci/bmaf022","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf022","url":null,"abstract":"Huangxueyishen decoction (HXYS) is proven effective in treating chronic renal failure in clinical practice. The study aims to identify and analyze the chemical constituents of HXYS decoction, and to quantitatively analyze and perform the study of the pharmacokinetics of its main active ingredients. The Ultra-Performance Liquid Chromatography-Linear Trap Quadrupole-Orbitrap Mass Spectrometry (UPLC-LTQ-Orbitrap-MS) system was used to qualitatively analyze the main components of HXYS. Among these compounds, UPLC-QTRAP-MS/MS was applied to further perform the simultaneous quantification of selected important constituents, and pharmacokinetic studies were performed on eight blood-entry components. A total of 87 compounds were tentatively identified, including 26 flavonoids and flavonoid glycosides, 9 phthalides, 9 phenylpropanoids, 9 lignans and 30 other compounds. Two rapid, sensitive and reliable UPLC-MS/MS method have been successfully developed for the simultaneous determination of 11 constituents and 8 components in the plasma of rats at different time points after HXYS administration. Tmax of the eight components was 0.88-4.00 h, t1/2 was 0.65 ~ 4.58 h and AUC(0-∞) ranged from 145.88 ~ 1785.63 μg·h/L. In this study, the chemical components of HXYS were comprehensively characterized, and the active components were further screened in combination with network pharmacology, which predicted and verified the chemical material basis of HXYS and laid the foundation for analyzing its bioactive substances.","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":"144020019","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}

引用次数: 0

Rapid Characterization and Identification of the Chemical Constituents in San-Huang-Xie-Xin-Tang, a Traditional Chinese Medicine Formula, by High Performance Liquid Chromatography Coupled to Electrospray Ionization and Quadrupole Time-of-Flight Mass Spectrometry. 高效液相色谱-电喷雾离子化和四极杆飞行时间质谱法快速表征和鉴定中药配方三黄解毒汤中的化学成分

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmae056

Lei Liu, Pei Hu, Mengmo Chen, Jiasi Huang, Qing Zhang, Yun Ling

{"title":"Rapid Characterization and Identification of the Chemical Constituents in San-Huang-Xie-Xin-Tang, a Traditional Chinese Medicine Formula, by High Performance Liquid Chromatography Coupled to Electrospray Ionization and Quadrupole Time-of-Flight Mass Spectrometry.","authors":"Lei Liu, Pei Hu, Mengmo Chen, Jiasi Huang, Qing Zhang, Yun Ling","doi":"10.1093/chromsci/bmae056","DOIUrl":"10.1093/chromsci/bmae056","url":null,"abstract":"San-Huang-Xie-Xin-Tang (SHXXT), a traditional Chinese medicine formula composed of Coptidis rhizome (CR), Scutellariae radix (SR) and Rhei rhizome (RR), is widely used to treat hypertension, gastritis and peptic ulcer clinically. However, the chemical constituent of SHXXT is still unclear due to its complexity, which hindered the discovery of effective compounds and quality control. Thus, an in-depth understanding of its chemical constituents is very essential. To address this problem, comprehensive analysis of chemical constituents of SHXXT was performed by high performance liquid chromatography coupled to electrospray ionization and quadrupole time-of-flight mass spectrometry (HPLC-ESI-QTOF-MS/MS). As a result, 45 compounds were identified, including 8 phenolic acids, 15 flavonoids, 13 alkaloids, 8 anthraquinones and 1 lignan. Among them, 17 compounds were from CR, 17 compounds were from SR and 11 compounds were from RR. This established method can systematically and rapidly analyze the chemical constituents in SHXXT, which provides chemical foundation for further research on effective substances and action mechanism of SHXXT.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142583067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Fast Determination of Propofol in Human Plasma Using C18-Functionalized Magnetic Nanomaterials Followed by Supercritical Fluid Chromatography. 利用 C18 功能化磁性纳米材料和超临界流体色谱法快速测定人血浆中的丙泊酚。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmae053

Shan-Yan Liang, Xiao-Min Xu, Peng Wang, Ming-Li Ye, Shui-Feng Zhang, Yong-Gang Zhao

{"title":"Fast Determination of Propofol in Human Plasma Using C18-Functionalized Magnetic Nanomaterials Followed by Supercritical Fluid Chromatography.","authors":"Shan-Yan Liang, Xiao-Min Xu, Peng Wang, Ming-Li Ye, Shui-Feng Zhang, Yong-Gang Zhao","doi":"10.1093/chromsci/bmae053","DOIUrl":"10.1093/chromsci/bmae053","url":null,"abstract":"Novel C18-functionalized magnetic nanomaterials; i.e., C18@poly-styrene-divinylbenzene-glycidyl methacrylate-Fe3O4 (C18@PS-DVB-GMA-Fe3O4) have been synthesized by using N, N-dimethyloctadecylamine as modifying agent, which could be beneficial to remove the blood phospholipids. The C18@PS-DVB-GMA-Fe3O4 nanoparticles have been used and evaluated in the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) procedure for human plasma prior to the analysis of propofol by supercritical fluid chromatography (SFC). In the QuEChERS procedure, human plasma samples are directly mixed with extraction solvent and C18@PS-DVB-GMA-Fe3O4 nanoparticles, and the extraction and cleanup procedures have been accomplished simultaneously. The SFC separation was performed with a C18 column (Thermo Scientific™ Acclaim™ 120, 250 × 4. 6 mm, 5 μm) within 5 min, using thymol as the internal standard. Supercritical carbon dioxide was used as the mobile phase with methanol as the cosolvent at the flow rate of 1.0 mL/min. The column temperature was 38°C, and detection wavelength was 275 nm. A good linearity was obtained among the propofol concentration range of 0.5-10 mg/L (R2 = 0.9997) with the limit of detection of 0.17 mg/L. Recoveries were in the range of 76.5-91.9%, with RSD less than 7.9%. These results suggested that method is convenient, rapid with high accuracy and little matrix effect, and suitable for rapid determination of propofol plasma concentration.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142466604","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Stability Indicating RP-HPLC Method by QbD Approach and LC-MS Characterization of Degradation Products of Mifepristone. QbD法测定米非司酮降解产物的反相高效液相色谱法及LC-MS表征。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf017

Chandni Chandarana, Isha Juwarwala, Parixit Prajapati, Jaimin Kumar Patel

{"title":"Stability Indicating RP-HPLC Method by QbD Approach and LC-MS Characterization of Degradation Products of Mifepristone.","authors":"Chandni Chandarana, Isha Juwarwala, Parixit Prajapati, Jaimin Kumar Patel","doi":"10.1093/chromsci/bmaf017","DOIUrl":"10.1093/chromsci/bmaf017","url":null,"abstract":"A Stability indicating revered phase high performance liquid chromatography (RP-HPLC) method have been developed and validated for the estimation of Mifepristone. LC-MS Studies was carried out for identification of possible degradation products. A simple, rapid, accurate and precise stability indicating RP-HPLC method was developed for quantification of Mifepristone. The developed method used the mixture of methanol and water (88:12 v/v) as mobile phase at flow rate of 1 ml /min, which was optimized with the help of Quality by Design approach. Detection was carried out at 305 mm. The linearity of the proposed method was found in the concentration range of 5-25 μg/ml with regression coefficient (R2) of 0.996. LOD and LOQ were found to be 0.0324 and 0.0982 μg/ml, respectively. The recovery of the proposed method was found to be 98%-100%. The method was found to be precise and robust. The developed stability indicating RP-HPLC method was successfully applied for quantification of Mifepristone in pharmaceutical dosage form. The degradation products were characterized by LC-MS and the fragmentation pathways were proposed.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143753008","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Universal Quantitative Residual Solvent Analysis of Solids and Liquids Using a Full Evaporative Technique and Methanized Flame Ionization Detection. 使用全蒸发技术和甲基化火焰电离检测的固体和液体残留溶剂的通用定量分析。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf014

Allison Ferranti, Taylor Hayward

{"title":"A Universal Quantitative Residual Solvent Analysis of Solids and Liquids Using a Full Evaporative Technique and Methanized Flame Ionization Detection.","authors":"Allison Ferranti, Taylor Hayward","doi":"10.1093/chromsci/bmaf014","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf014","url":null,"abstract":"Residual solvent analysis is a common method used in the manufacturing of finished goods and pharmaceuticals to ensure the safety of the final product to the consumer. Typically, this involves a headspace sample introduction set up and then separation by gas chromatography (GC) with detection by a flame ionization detector (FID). This analysis can be very time consuming in sample preparation, calibration and analysis time. A full evaporative technique has been applied to both solid and liquid samples for the rapid vaporization of the solvent analytes, which is then introduced to a GC for separation. Additionally, a methanizer was used in line with the FID creating a uniform response for solvents of various heteroatoms and functionalities. This combination of full evaporative technique with a methanized-FID allows for the use of a single response factor for residual solvent analysis with demonstrated repeatability of ˂4%RSD. Spiked solid sample analysis shows recovery between 95% and 105% of solvents tested at ⁓2 μg of each analyte. Overall, the combination of full evaporative headspace sampling and methanized-FID can be applied to any sample matrix for any solvent used in manufacturing or production, making a universal method for residual solvent analysis.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730251","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

RP-HPLC Method Development and Validation for Simultaneous Estimation of Berberine and Ursolic Acid in Formulation. 反相高效液相色谱法测定制剂中小檗碱和熊果酸含量的建立及验证。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf016

Vineeta V Khanvilkar, Shruti S Mandle, Prachi R Hande, Bhavin R Daka, Pratik P Jadhav

{"title":"RP-HPLC Method Development and Validation for Simultaneous Estimation of Berberine and Ursolic Acid in Formulation.","authors":"Vineeta V Khanvilkar, Shruti S Mandle, Prachi R Hande, Bhavin R Daka, Pratik P Jadhav","doi":"10.1093/chromsci/bmaf016","DOIUrl":"10.1093/chromsci/bmaf016","url":null,"abstract":"Medicines used in ayurveda are typically made of many herbs or are polyherbals. Standardization of these medicines can be carried out by quantitative estimation of two or more of its markers simultaneously. Berberine and ursolic acid are two active markers which are present in an Ayurvedic formulation, Giloy Tulsi tablets. In the present research work, the Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the simultaneous quantitative determination of berberine and ursolic acid from the formulation. With an RP Hemochrom C18 column, chromatographic separation was accomplished at 292 nm with eluent composed of methanol: acetonitrile (4:1, v/v) at a flow rate of 1.0 mL/min. The retention time of berberine and ursolic acid was obtained to be 1.5 ± 0.02 and 3.2 ± 0.02 min, respectively. A simple, rapid, accurate, specific, and robust analytical method was developed to estimate berberine and ursolic acid. This validated method can be used for routine quality control of ayurvedic formulations or herbal formulations having plants which contain berberine and ursolic acid.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730255","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0