Journal of chromatographic science最新文献

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Chemical Profiling of Shen-Wu-Yi-Shen Tablets Using UPLC-Q-TOF-MS/MS and Its Quality Evaluation Based on UPLC-DAD Combined with Multivariate Statistical Analysis. 基于UPLC-DAD结合多元统计分析的UPLC-Q-TOF-MS/MS神武一味片化学成分分析及其质量评价
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmae001
Yudan Mei, Yumei Hu, Xiaoqian Tao, Jing Shang, Mengyu Qian, Fengtai Suo, Jifeng Li, Liang Cao, Zhenzhong Wang, Wei Xiao
{"title":"Chemical Profiling of Shen-Wu-Yi-Shen Tablets Using UPLC-Q-TOF-MS/MS and Its Quality Evaluation Based on UPLC-DAD Combined with Multivariate Statistical Analysis.","authors":"Yudan Mei, Yumei Hu, Xiaoqian Tao, Jing Shang, Mengyu Qian, Fengtai Suo, Jifeng Li, Liang Cao, Zhenzhong Wang, Wei Xiao","doi":"10.1093/chromsci/bmae001","DOIUrl":"10.1093/chromsci/bmae001","url":null,"abstract":"<p><p>Shen-Wu-Yi-Shen tablets (SWYST) is a traditional Chinese medicine prescription used for treating chronic kidney disease (CKD). This study aims to characterize the constituents in SWYST and evaluate the quality based on the quantification of multiple bioactive components. SWYST samples were analyzed with ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and a data-processing strategy. As a result, 215 compounds in SWYST were unambiguously identified or tentatively characterized, including 14 potential new compounds. Meanwhile, strategies based on characteristic fragments for rapid identification were summarized, indicating that the qualitative method is accurate and feasible. Notably, the glucose esters of laccaic acid D-type anthraquinone were first found and their fragmentation patterns were described by comparing that of O-glycoside isomers. Besides, based on comparisons of the cleavage ways of mono-acyl glucose with different acyl groups or acylation sites, differences in fragmentation pathways between 1,2-di-O-acyl glucose and 1,6-di-O-acyl glucose were proposed for the first time and verified by reference substances. In addition, a validated UPLC-DAD was established for the determination of 11 major bioactive components related to treatment of CKD (albiflorin, paeoniflorin, 2,3,5,4'-tetrahydroxy-stilbene-2-O-β-d-glucoside (TSG), 1-O-galloyl-2-O-cinnamoyl-β-d-glucose, emodin-8-O-β-d-glucoside, chrysophanol-O-β-d-glucoside, aloe-emodin, rhein, emodin, chrysophanol and physcion). Moreover, TSG and 1-O-galloyl-2-O-cinnamoyl-β-d-glucose were found as the quality markers related to the origins of SWYST based on multivariate statistical analysis. Conclusively, the findings in this work provide a feasible reference for further studies on quality research and mechanisms of action in treating CKD.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"534-553"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139512453","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
Theoretical Study of Non-Isothermal Gradient Elution Liquid Chromatography. 非等温梯度洗脱液相色谱法的理论研究
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad076
Nazia Rehman, Ayesha Parveen, Shamsul Qamar
{"title":"Theoretical Study of Non-Isothermal Gradient Elution Liquid Chromatography.","authors":"Nazia Rehman, Ayesha Parveen, Shamsul Qamar","doi":"10.1093/chromsci/bmad076","DOIUrl":"10.1093/chromsci/bmad076","url":null,"abstract":"<p><p>A two-component model of gradient elution chromatography is investigated to theoretically study the effects of simultaneous variations in temperature and solvent strength on the retention behaviors of elution profiles in thermally insulated liquid chromatographic columns. The gradient elution technique is based on the gradual increase or decrease in eluent strength during the chromatographic operation by varying the composition of the mobile phase. The enthalpy of adsorption is primarily responsible for internal temperature variations inside the column, as heat adsorbs during the adsorption process and releases in the desorption phase. Both types of variations change the propagation speeds of moving pulses inside the column which can lead to better separation of the components and a reduction in the recycling time for the next injection. The equilibrium dispersive model (EDM) coupled with the energy balance equation for temperature and transport equation for the volume fraction of the solvent is utilized to simulate this complex process. The resulting nonlinear model equations are approximated by applying a semi-discrete second-order finite volume scheme. The numerical solutions are used to study the impact of a gradient starting and ending times, volume-fraction of the solvent, solvent strength parameter, the slope of gradient, enthalpy of adsorption, injection temperature, and the ratio of specific heats on the concentration profiles.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"515-525"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10554334","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
Determination of 11 Kinds of Hair Dyes in Hair-Dyeing Products by Liquid Chromatography-Tandem Mass Spectrometry. 利用液相色谱-串联质谱法测定染发产品中的 11 种染发剂。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad071
Yu-Xiang Gu, Li-Song Chen, Lei Nie
{"title":"Determination of 11 Kinds of Hair Dyes in Hair-Dyeing Products by Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Yu-Xiang Gu, Li-Song Chen, Lei Nie","doi":"10.1093/chromsci/bmad071","DOIUrl":"10.1093/chromsci/bmad071","url":null,"abstract":"<p><p>Eleven kinds of hair dyes were determined in hair-dyeing products by liquid chromatography-tandem mass spectrometry (MS). The samples were extracted with ultrasound in methanol for 20 min. After centrifugation, the supernatant was diluted with 10% methanol/90% water (v/v). Then, the solution was analyzed by Shim-pack Scepter C18-120 column (100 mm × 2.1 mm, 1.9 μm) plus electrospray ionization-MS/MS. Matrix-matched standard solutions were used to analyze the samples. The limits of detection were from 0.15 to 10 mg/kg, the limits of quantification were from 0.5 to 40 mg/kg and the recovery was from 79.4 to 109.2%. The protocol was selective and accurate and was satisfyingly applied to analyze hair dyes in different kinds of commercial products. 1-Hydroxyethyl-4,5-diaminopyrazole sulfate, hydroxyethyl-p-phenylenediamine sulfate, 2-methyl-5-hydroxyethylaminophenol, 5-amino-6-chloro-o-cresol, 3-nitro-p-hydroxyethylaminophenol and 2-amino-6-chloro-4-nitrophenol were detected in 10 samples with the concentrations between limits of detection and quantification to 9.27 × 104 mg/kg.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"499-507"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10439694","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 of Relatively Simple Sample Pretreatment Strategies to Selectively Remove Chromatographic Interfering Peaks of Polysorbate 80 from Liquid Oral Finished Drug Product. 开发相对简单的样品预处理策略,从液体口服药物成品中选择性去除聚山梨醇酯 80 的色谱干扰峰。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad064
Sarju Adhikari, Shane N Berger, Abu M Rustum
{"title":"Development of Relatively Simple Sample Pretreatment Strategies to Selectively Remove Chromatographic Interfering Peaks of Polysorbate 80 from Liquid Oral Finished Drug Product.","authors":"Sarju Adhikari, Shane N Berger, Abu M Rustum","doi":"10.1093/chromsci/bmad064","DOIUrl":"10.1093/chromsci/bmad064","url":null,"abstract":"<p><p>Polysorbate 80 (PS 80) is a nonionic surfactant, used in myriad of pharmaceutical, food and cosmetic formulations. PS 80 components have strong UV absorbance and retain under reversed-phase chromatographic conditions, significantly masking sections of the chromatogram. PS 80-related peaks interferences in a sample are common and can be difficult to separate from the analyte peaks. A liquid oral finished product (LOFP) containing PS 80 and Ivermectin as the active pharmaceutical ingredient (API) was selected for this study. Herein, we report two sample pretreatment strategies focusing on the selective removal of PS 80 from the LOFP. Both methods significantly reduce and/or practically eliminate excipients and PS 80-related peaks interferences from the LOFP without a negative impact on the API and its key-related substances recovery. The solid-phase extraction (SPE) strategy uses a C18 SPE followed by a silica gel SPE, whereas the liquid-liquid extraction strategy uses in situ-generated sodium caprylate for the removal of formulation excipients and PS 80. These methods can significantly increase the reliability of high-performance liquid chromatography methods and decrease false positive out-of-specifications events because of coelution of PS 80-related peaks with peaks of interest.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"593-599"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10018715","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 of HPLC-UV Method for Simultaneous Determination of Corticosteroid Co-Administered Immune Therapy. 开发用于同时测定皮质类固醇联合免疫疗法的高效液相色谱-紫外法。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad050
Nessreen S Abdelhamid, Nehal F Farid, Basma H Anwar, Maimana A Magdy
{"title":"Development of HPLC-UV Method for Simultaneous Determination of Corticosteroid Co-Administered Immune Therapy.","authors":"Nessreen S Abdelhamid, Nehal F Farid, Basma H Anwar, Maimana A Magdy","doi":"10.1093/chromsci/bmad050","DOIUrl":"10.1093/chromsci/bmad050","url":null,"abstract":"<p><p>Prednisolone (PDS) has recently been utilized to treat a variety of medical disorders, including autoimmune illnesses and cancer. It is also used to treat coronavirus disease 2019 infection-related respiratory problems. Because it may induce health problems including gastrointestinal lesions and ulceration, it has to be used alongside other drugs like esomeprazole (ESM), which acts as a proton pump antagonist to reduce the probability of ulceration. As a result, the goal of this research is to create an environmentally safe and sensitive high-performance liquid chromatography (HPLC) approach for determining PDS and ESM in their binary combination and spiked human plasma. C8 column (100 × 4.6 mm, 5 μm) and gradient mobile phase elution were used to separate the studied drugs with ultraviolet recognition at 290 nm. Caffeine was utilized as an internal standard to adjust the sample variance. Plasma, caffeine, ESM and PDS all had tR values of 1.4, 3.5, 6.3 and 7.3, respectively. The suggested method's greenness features were evaluated using three greenness evaluation tools: green analytical procedure index, analytical greenness metric approach and analytical eco-scale, and the findings were approved and satisfied. Validation parameters were evaluated in accordance with US-FDA recommendations in order to meet the global desires for biological analysis technique, acceptable limits were obtained.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"554-561"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10195846","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
Central Composite Design Expert-Supported RP-HPLC Optimization and Quantitative Evaluation of Efonidipine Hydrochloride Ethanolate & Chlorthalidone in Tablet. 中央配合物设计专家支持的RP-HPLC法优化和定量评价盐酸埃夫尼地平片中乙醇和氯噻酮的含量。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad077
Bhoomi D Patel, Hitesh J Vekaria
{"title":"Central Composite Design Expert-Supported RP-HPLC Optimization and Quantitative Evaluation of Efonidipine Hydrochloride Ethanolate & Chlorthalidone in Tablet.","authors":"Bhoomi D Patel, Hitesh J Vekaria","doi":"10.1093/chromsci/bmad077","DOIUrl":"10.1093/chromsci/bmad077","url":null,"abstract":"<p><p>Central composite design based RP-HPLC method optimization for the synchronized analysis of Efonidipine Hydrochloride Ethanolate (EFE) and Chlorthalidone (CHL) in tablet. The effective separation was performed using Inertsil ODS C18 column (250 × 4.6 mm, 5 μm), PDA detector with 0.05 M KH2PO4 Buffer (pH 4.5): Acetonitrile (40:60%v/v) mobile phase. Independent variables were investigated include the concentration of KH2PO4 (X1) and flow rate of mobile phase (X2). Based on responses obtained (retention time, resolution and tailing factor), the optimum condition selected was X1 = 40% and X2 = 1 ml/min. Optimized HPLC condition was validated by assessing validation parameters and it meets the acceptance criteria set by ICH. The linear calibration curve was found to be in the quantity range 6.25-18.75 and 20-60 μg/ml Assay of drugs was 100.94 and 100.06% for CHL and EFE. The validated RP-HPLC-PDA method can be used for routine analysis of EFE and CHL in tablet.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"585-592"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41127205","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
Experimental Design Application for Measuring Histamine in Tuna Fish Samples by Phenyl Isothiocyanate Derivation Method Using Ultra-Performance Liquid Chromatography. 利用超高效液相色谱法的异硫氰酸苯酯衍生法测定金枪鱼样品中组胺的实验设计应用
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad060
Maede Ameri, Seyed Mosayeb Daryanavard
{"title":"Experimental Design Application for Measuring Histamine in Tuna Fish Samples by Phenyl Isothiocyanate Derivation Method Using Ultra-Performance Liquid Chromatography.","authors":"Maede Ameri, Seyed Mosayeb Daryanavard","doi":"10.1093/chromsci/bmad060","DOIUrl":"10.1093/chromsci/bmad060","url":null,"abstract":"<p><p>Histamine as an important biogenic amino acid was measured in tuna fish samples by ultra-performance liquid chromatography using a phenyl isothiocyanate derivative. Minitab software was used to design the experiment and investigate the effective factors during the process, which includes screening and optimization steps. A partial factorial design was used in the screening stage and a central composite design was used in the optimization. Effective parameters in histamine derivatized were examined in the screening step including triethylamine volume, phenyl isothiocyanate volume, reaction temperature, reaction time and mobile phase pH. Then, in the optimization, effective parameters were identified and finally, the calibration curve was drawn from a concentration of 0.5-10.0 μg.mL-1 for histamine derivatized and a correlation coefficient of 0.994 was obtained for histamine derivatized. The method detection limit was 0.36 μg.mL-1 and the limit of quantification (LOQ) was 1.19 μg.mL-1. The relative standard deviation of the method was obtained for concentrations of 1.0-100.0 μg.mL-1 in the range between 1.06 and 2.21%. The recovery method was obtained from 90.8 to 103.1% for measuring histamine derivatized in real fish samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"570-579"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9923949","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
Simultaneous Determination of Thirteen Iridoid Glycosides in Crude and Processed Fructus Corni from Different Areas by UPLC-MS/MS Method. UPLC-MS/MS法同时测定不同产地山茱萸粗品和加工品中13种鸢尾苷的含量。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-07-10 DOI: 10.1093/chromsci/bmad083
Fan Zhang, Yu Yan, Jie-Kun Xu, Lin-Mei Zhang, Li Li, Xin Chen, Dong-Xu Li, Ying Peng, Hua Yang, Ling-Zhi Li, Jun He, Jiang Zheng, Wei-Ku Zhang
{"title":"Simultaneous Determination of Thirteen Iridoid Glycosides in Crude and Processed Fructus Corni from Different Areas by UPLC-MS/MS Method.","authors":"Fan Zhang, Yu Yan, Jie-Kun Xu, Lin-Mei Zhang, Li Li, Xin Chen, Dong-Xu Li, Ying Peng, Hua Yang, Ling-Zhi Li, Jun He, Jiang Zheng, Wei-Ku Zhang","doi":"10.1093/chromsci/bmad083","DOIUrl":"10.1093/chromsci/bmad083","url":null,"abstract":"<p><p>Fructus Corni (F. Corni) is the dried mature pulp of Cornus officinalis Sieb. et Zucc.(Cornaceae), which is rich in iridoids. In this study, a simple, sensitive and rapid UPLC-MS/MS method was developed for the simultaneous determination of 13 iridoid glycosides of F. Corni from different areas. Specifically, we included five new compounds (cornusdiridoid C, cornusdiridoid E, cornusdiridoid F, 3'',5''-dehydroxycornuside and 2'-O-p-coumaroyl-kingiside) and isomers (2'-O-p-E-coumaroylloganin and 2'-O-p-Z-coumaroylloganin) for the first time in the quality markers of F. Corni. A total of 13 compounds and two pairs of isomers were well isolated and tested within just 14 min. All calibration curves showed good linear regression (r2 ≥ 0.99) within the tested concentration ranges. The limit of detection and limit of quantification were in the range of 0.19-1.90 and 0.38-3.76 ng/mL, respectively. The intra-day and inter-day precision were <3.21% and 12.49%, the RSD values of repeatability did not exceed 6.81% and the average recoveries were 90.95-113.59% for the analytes. All iridoid glycosides stabilized within 12 h (RSD < 10.99%). This method has been successfully applied to the quality evaluation of crude and processed F. Corni from different areas. The determination of characteristic iridoid glycosides and isomers will provide a more reliable and comprehensive method for the evaluation of F. Corni.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"562-569"},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49690732","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
Problems in Commercial Kits of 25-Hydroxy Vitamin D and the Development of Simple, Robust and Faster HPLC Method. 25-Hydroxy Vitamin D 商用试剂盒中存在的问题以及简单、稳健、快速的 HPLC 方法的开发。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-06-23 DOI: 10.1093/chromsci/bmae042
Syed Muhammad Saad, Abdul Rafiq Khan, Khalid Mohammed Khan, Ali Al-Othaim
{"title":"Problems in Commercial Kits of 25-Hydroxy Vitamin D and the Development of Simple, Robust and Faster HPLC Method.","authors":"Syed Muhammad Saad, Abdul Rafiq Khan, Khalid Mohammed Khan, Ali Al-Othaim","doi":"10.1093/chromsci/bmae042","DOIUrl":"https://doi.org/10.1093/chromsci/bmae042","url":null,"abstract":"<p><p>Vitamin D is a lipid-soluble compound that plays a key role in bone mineral metabolism. The commercial current kits and several published assay methods (High-performance liquid chromatography (HPLC) and Immunoassay) are complicated due to the use of multiple reagents, larger sample volume, high backpressure, longer extraction time, evaporation under nitrogen after extraction, significant interference and antibody cross-reactivity. Here we report a new HPLC method for the determination of 25-hydroxyvitamin D2 (25-OHD2) and 25-hydroxyvitamin D3 (25-OHD3) that is simple (no evaporation), rapid (10-minute run time) and robust. Serum sample (300 μl) is mixed with 300 μl acetonitrile containing lauraphenone as internal standard. After vortexing and centrifugation, the supernatant was loaded into C18 extraction cartridges, washed with 70% methanol and then eluted with 200 μl of a mixture of 70% ethanol and 30% isopropyl alcohol (IPA). The eluent was mixed with 50 μl of water and injected into the HPLC-UV system for analysis. The method proved to be linear in the range of 10-750 nmol/L of 25-OHD2 and 25-OHD3. The intra- and inter-assay precision was less than 10 for both compounds at four different concentrations. The method was compared with (LC-MS/MS) and the correlation coefficients (R2) were 0.9454 and 0.9673 for 25-OHD2 and 25-OHD3 respectively. The proposed HPLC method is simple, rapid, robust and free from the most common problems encountered with commercial kits. It can be used in a high-volume laboratory that uses the HPLC method for the simultaneous determination of 25-OHD2 and 25-OHD3 in serum samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2024-06-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141442784","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
Structural Elucidation of Novel Degradation Impurity and Development, Validation of a Single HPLC Method for all Putative Impurities of Clobetasol Propionate in a Foam Drug Product. 新型降解杂质的结构阐释以及针对泡沫药物产品中丙酸氯倍他索所有假定杂质的单一高效液相色谱法的开发和验证。
IF 1.3 4区 化学
Journal of chromatographic science Pub Date : 2024-05-31 DOI: 10.1093/chromsci/bmad016
Naga Venkata Durga Prasad Ketha, Deepti Kolli, Praveen Kumar Subbappa
{"title":"Structural Elucidation of Novel Degradation Impurity and Development, Validation of a Single HPLC Method for all Putative Impurities of Clobetasol Propionate in a Foam Drug Product.","authors":"Naga Venkata Durga Prasad Ketha, Deepti Kolli, Praveen Kumar Subbappa","doi":"10.1093/chromsci/bmad016","DOIUrl":"10.1093/chromsci/bmad016","url":null,"abstract":"<p><p>Clobetasol Propionate is a highly strong corticosteroid that is used in a variety of topical medication formulations, including foam, ointment, lotion, spray and shampoo; with a dosage strength of 0.05% (w/w). The goal of this research was to identify and characterize a substantial unknown impurity (UK) detected during the stability testing of a Clobetasol Propionate foam pharmaceutical product in accelerated conditions (40°C and 75% relative humidity). Developing a single, robust and accurate HPLC method that is LC-MS compatible for quantifying all 14 potential Clobetasol Propionate impurities in therapeutic drugs is another goal. Preparative column chromatography was used to separate the impurity, and spectroscopic techniques like IR, NMR and MS were used to characterize its structure. The structure of isolated UK was effectively characterized and defined using spectroscopic data evaluation. The chromatographic method has also been validated according to the International Conference on Hominization's Q (2) quality guidelines. The isolated and characterized impurity had the same equivalence as the impurity found during stability testing. Precision, accuracy, linearity, robustness and ruggedness are all met in the method validation data.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"444-453"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10814377","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
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