Journal of chromatographic science最新文献

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A GC–MS Method for Determination of β-Propiolactone Residues in Inactivated Covid-19 Vaccines 测定灭活 Covid-19 疫苗中 β-丙内酯残留量的气相色谱-质谱方法
IF 1.3 4区 化学
Journal of chromatographic science Pub Date : 2024-09-17 DOI: 10.1093/chromsci/bmae049
Seyedeh Zohreh Mirjalili, Zahra Tamiji, Mehrnoosh Shirangi, Mohsen Amini
{"title":"A GC–MS Method for Determination of β-Propiolactone Residues in Inactivated Covid-19 Vaccines","authors":"Seyedeh Zohreh Mirjalili, Zahra Tamiji, Mehrnoosh Shirangi, Mohsen Amini","doi":"10.1093/chromsci/bmae049","DOIUrl":"https://doi.org/10.1093/chromsci/bmae049","url":null,"abstract":"β-propiolactone is a common inactivator agent used in vaccines. Due to β-propiolactone carcinogenicity, complete hydrolysis of it is necessary to prevent cytotoxicity in mammalian cells. As a result, more attention should be paid to it at the clinic, and it is important to measure its trace amounts. β-propiolactone analysis is challenging due to its instability. A simple and fast gas chromatography–mass spectrometry method was developed for quantitation of residual β-propiolactone in inactivated coronavirus disease 2019 (Covid-19) vaccines. Caprolactone was used as an internal standard in sample solutions; the analysis was performed after extraction of analyte from vaccine media by ethyl acetate. The validity of the method was studied with a linearity of r2 > 0.99 over the concentration range of 0.2–20 μg/mL with the limit of detection and the limit of quantification of 0.07 and 0.20 μg/mL, respectively. The target analyte β-propiolactone was not detected in the samples, demonstrating the test samples were qualified. The established method can be used for quality control of inactivated Covid-19 vaccines.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142264533","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
Ayurveda Detoxification Process Reduces Plumbagin from the Roots of Plumbago zeylanica L. - A RP-UFLC Analysis. 阿育吠陀排毒过程减少了 Plumbago zeylanica L. 根中的 Plumbagin - RP-UFLC 分析。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-09-06 DOI: 10.1093/chromsci/bmae048
Gireesh M Ankad, Harsha Hegde, Iranna B Kotturshetti
{"title":"Ayurveda Detoxification Process Reduces Plumbagin from the Roots of Plumbago zeylanica L. - A RP-UFLC Analysis.","authors":"Gireesh M Ankad, Harsha Hegde, Iranna B Kotturshetti","doi":"10.1093/chromsci/bmae048","DOIUrl":"https://doi.org/10.1093/chromsci/bmae048","url":null,"abstract":"<p><p>Ayurveda describes purification process of certain herbal drugs to reduce the toxicity and make them suitable for therapeutic purpose. The objective of the study was to evaluate the effect of detoxification process on plumbagin (PG) from the Plumbago zeylanica L. roots in marketed samples. It involved procurement of market samples from five states of India viz. Andhra Pradesh, Gujarat, Maharashtra, Madhya Pradesh and Punjab. The roots were purified in lime water (LW) as mentioned in Ayurveda. Reverse Phase Ultra-Flow Liquid Chromatography method was validated for identification of PG in unprocessed and processed roots and in the media (LW) used for purification after processing. The data was statistically analyzed by Analysis of Variance (ANOVA) and tested for significance by the Dunnett multiple comparison test. Results were expressed as mean ± SD mg/g dry weight of extract. The study indicated that the PG was reduced quantitatively after processing, while the amount of PG found in the LW was observed to be increased, indicating the leaching of PG during the purification process. In conclusion, the detoxification process eliminates PG from its roots and discloses the leaching effect in the media for the first time.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-09-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142140263","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 General Active Ingredients in Topical Formulations by Gas Chromatography with Flame Ionization Detection (GC-FID). 气相色谱-火焰离子化检测器(GC-FID)同时测定外用制剂中一般有效成分。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmad086
Anna Ioutsi, Anastasia Sarnitskaya, Mikhail Sumtsov
{"title":"Simultaneous Determination of General Active Ingredients in Topical Formulations by Gas Chromatography with Flame Ionization Detection (GC-FID).","authors":"Anna Ioutsi, Anastasia Sarnitskaya, Mikhail Sumtsov","doi":"10.1093/chromsci/bmad086","DOIUrl":"10.1093/chromsci/bmad086","url":null,"abstract":"<p><p>A simple, fast, precision and sensitive gas chromatographic method was developed for determination of camphor, L-menthol, methyl salicylate, salicylic acid, benzyl nicotinate and nonivamide in topical formulations. The possibility of determination low-boiling components and high-boiling components by a single analytical method was shown. The method was optimized by evaluating the effect of a large number of chromatographic parameters and sample preparation stages. It was validated according to the International Council on Harmonization guidelines. Limit of quantification of active components were achieved from 0.7 μg/mL for benzyl nicotinate and L-menthol to 41 μg/mL for salicylic acid. High repeatability and good recovery values were demonstrated. The practical application of the proposed method was shown for ointments and cream.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"107591426","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 Quantification of Vancomycin, Linezolid and Voriconazole in Human Plasma by UHPLC-MS/MS: Application in Therapeutic Drug Monitoring. 超高效液相色谱-质谱/质谱法同时定量测定人血浆中的万古霉素、利奈唑胺和伏立康唑:在治疗药物监测中的应用
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmae017
Yao Liu, Yanan Li, Wenli Chen, Dandan Ming, Wenji Luo, Jiabi Liang
{"title":"Simultaneous Quantification of Vancomycin, Linezolid and Voriconazole in Human Plasma by UHPLC-MS/MS: Application in Therapeutic Drug Monitoring.","authors":"Yao Liu, Yanan Li, Wenli Chen, Dandan Ming, Wenji Luo, Jiabi Liang","doi":"10.1093/chromsci/bmae017","DOIUrl":"10.1093/chromsci/bmae017","url":null,"abstract":"<p><strong>Objective: </strong>Individual differences challenge the treatment of vancomycin, linezolid and voriconazole in severe infections. This study aimed to build a simple and economical method for simultaneous determination of the three antibiotics in human plasma by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and provided a reference for therapeutic drug monitoring (TDM) of infected patients.</p><p><strong>Methods: </strong>The plasma samples were precipitated by acetonitrile and detected and separated on a shim-pack GIST C18 column following the gradient elution within 5 min. Mass quantification was performed on multiple reaction monitoring mode under positive electrospray ionization.</p><p><strong>Results: </strong>The linear ranges of vancomycin, linezolid and voriconazole were 1.00-100.00, 0.10-15.00 and 0.10-20.00 μg·mL-1, respectively, with good linearity (R2 > 0.99). The accuracy and precision, matrix effect, extraction recovery and stability were validated, and the results all meet the acceptance criteria of China Food and Drug Administration (CFDA) guidelines.</p><p><strong>Conclusion: </strong>The UHPLC-MS/MS method was established and validated for the simultaneous determination of vancomycin, linezolid and voriconazole in human plasma and successfully applied to routine TDM for individualized treatment.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140898504","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
Green and Sustainable Analytical Chemistry-Driven Chromatographic Method Development for Stability Study of Apixaban Using Box-Behnken Design and Principal Component Analysis. 利用盒-贝肯设计和主成分分析法,为阿哌沙班的稳定性研究开发绿色和可持续的分析化学驱动色谱方法
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmad033
Pintu Prajapati, Pooja Rajpurohit, Veera Shakar Pulusu, Shailesh Shah
{"title":"Green and Sustainable Analytical Chemistry-Driven Chromatographic Method Development for Stability Study of Apixaban Using Box-Behnken Design and Principal Component Analysis.","authors":"Pintu Prajapati, Pooja Rajpurohit, Veera Shakar Pulusu, Shailesh Shah","doi":"10.1093/chromsci/bmad033","DOIUrl":"10.1093/chromsci/bmad033","url":null,"abstract":"<p><p>Apixaban (APX) is a novel anti-coagulant drug approved by USFDA. According to referred literature, numerous chromatographic methods such as RP-HPLC and high-performance thin-layer chromatography have been published for the stability study of APX. But these chromatographic methods have been developed using toxic organic solvents that are hazardous to the environment and unsafe for analysts. Hence, green and sustainable analytical chemistry-driven chromatographic method has been developed for the stability study of APX using safe organic solvents for the safety of analysts and the protection of the environment. APX was subjected to forced degradation for the development of a stability-indicating assay method. The method development was carried out by the implementation of chemometric and DoE approaches for minimizing solvent wastage. Principal component analysis was applied for the identification of critical method risk variables (MRVs) and method performance attributes. DoE-based response surface modelling was applied for the optimisation of critical MRVs. The greenness profile scales of published and developed chromatographic methods have been assessed by NEMI and AGREE methods for the estimation of APX. The developed method was found to be more eco-friendly and robust than the published chromatographic methods for the estimation of APX.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9426873","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
Effects of Different Storage Times on the Stability of 12 Traditional Chinese Medicine Decoction Pieces. 不同储存时间对 12 味中药煎剂稳定性的影响
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmae030
Rui-Fang Xie, Yi-Ming Feng, Shan-Ni Li, Wei-Song Kong, Gui Zhou, Xin Zhou
{"title":"Effects of Different Storage Times on the Stability of 12 Traditional Chinese Medicine Decoction Pieces.","authors":"Rui-Fang Xie, Yi-Ming Feng, Shan-Ni Li, Wei-Song Kong, Gui Zhou, Xin Zhou","doi":"10.1093/chromsci/bmae030","DOIUrl":"10.1093/chromsci/bmae030","url":null,"abstract":"<p><p>As storage time increases, the quality of traditional Chinese medicines (TCMs) may change, and stability is an essential aspect of ensuring the safety and efficacy of TCMs. In this study, the effects of different storage times on the stability of 12 decoction pieces were evaluated. High-performance liquid chromatography was used to determine the contents of the active components in the 12 decoction pieces. The chemical composition data were analyzed using fingerprinting and clustering heatmap (CH). Results showed that during storage, significant variations (relative standard deviation > 10%) were observed in the levels of paeoniflorin in Paeoniae Radix Alba and Paeoniae Radix Rubra, hesperidin in Citri Reticulatae Pericarpium and Citri Reticulatae Pericarpium Viride, bufothionine in Siccus Bufo and chlorogenic acid in White Chrysanthemi Flos and Lonice Raejaponicae Caulis. However, calycosin-7-glucoside and calycosin in Astragali Radix Praeparata Cum Melle and chlorogenic acid in Lonicerae Japonicae Flos, Yellow Chrysanthemi Flos and Mori Folium were all <10%, which is consistent with the CH. Decoction pieces can be stored for up to six months, but it is recommended that volatile oil-containing and animal-based decoction pieces should not be stored for more than one month. This study provides new perspectives for the stability and quality control studies of TCM.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140945047","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
Comprehensive Quality Evaluation of Danggui-Jianzhong Decoction by Fingerprint Analysis, Multi-Component Quantitation and UPLC-Q-TOF-MS. 利用指纹图谱分析、多组分定量和UPLC-Q-TOF-MS对当归建中煎剂进行综合质量评价
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmae034
Lanyi Huang, Qing Liu, Wenfang Zhang, Bishan Lin, Yongjian Gao, Hong Deng, Shu Zhang
{"title":"Comprehensive Quality Evaluation of Danggui-Jianzhong Decoction by Fingerprint Analysis, Multi-Component Quantitation and UPLC-Q-TOF-MS.","authors":"Lanyi Huang, Qing Liu, Wenfang Zhang, Bishan Lin, Yongjian Gao, Hong Deng, Shu Zhang","doi":"10.1093/chromsci/bmae034","DOIUrl":"10.1093/chromsci/bmae034","url":null,"abstract":"<p><p>Danggui-Jianzhong decoction (DGJZ) is a famous classical traditional Chinese medicine formula, which ingredients are complex and the quality is difficult to control. Our study aimed to identify the overall chemical profile of DGJZ qualitatively by ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and UPLC. A total of 77 components, including terpenoids, flavonoids, phenolic acids, gingerols and other components, were firstly detected and characterized by UPLC-Q-TOF-MS and 18 peaks marked after analyzing the UPLC fingerprint. Finally, paeoniflorin, liquiritin, ferulic acid, cinnamic acid, glycyrrhizic acid and 6-gingerol were quantified, which was validated in terms of linearity, precision, accuracy, repeatability and recovery. Taken together, the chemical constitutes of DGJZ were systematically identified and a reliable quantitative method coupled with fingerprint analysis was successfully employed for evaluating the holistic quality, which will provide a robust foundation for the quality control of DGJZ.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141179597","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
Design of Experiment-Based Green UPLC-DAD Method for the Simultaneous Determination of Indacaterol, Glycopyrronium and Mometasone in their Combined Dosage Form and Spiked Human Plasma. 基于实验设计的绿色 UPLC-DAD 法同时测定茚达特罗、甘草酸铵和莫美他松的复方制剂和加标人体血浆。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmad072
Mohamed Tarek, Nermine S Ghoniem, Maha A Hegazy, Hebatallah A Wagdy
{"title":"Design of Experiment-Based Green UPLC-DAD Method for the Simultaneous Determination of Indacaterol, Glycopyrronium and Mometasone in their Combined Dosage Form and Spiked Human Plasma.","authors":"Mohamed Tarek, Nermine S Ghoniem, Maha A Hegazy, Hebatallah A Wagdy","doi":"10.1093/chromsci/bmad072","DOIUrl":"10.1093/chromsci/bmad072","url":null,"abstract":"<p><p>Indacaterol, is an ultra-long-acting β2 agonist, glycopyrronium is a long-acting muscarinic-antagonist and mometasone is a synthetic corticosteroid. They were used recently in combination for the treatment of severe asthma symptoms and chronic obstructive pulmonary disease. In this work, it was the first time to develop a green and environment friendly ultra-performance liquid chromatographic method using design expert program for the analysis of the three drugs in their combined dosage form. Also, the method was bioanalytically validated for the analysis of the three drugs in spiked human plasma samples. The method was linear in range from 0.50 to 100.0 μg mL-1 for indacaterol and mometasone and from 1.0 to 150.0 μg mL-1 for glycopyrronium. It showed high accuracy where, the % recovery for indacaterol, glycopyrronium and mometasone in plasma were ranged from 94.27 to 97.86%, 96.43 to 98.75% and 96.86 to 98.43%, respectively. Also, it was precise where, the % relative standard deviation for the inter-day precision was ranged from 2.571 to 3.484%, 3.180 to 4.123% and 3.150 to 3.984% and the intra-day precision was ranged from 2.351 to 3.125%, 2.512 to 3.544% and 2.961 to 3.983% for indacaterol, glycopyrronium and mometasone, respectively. The limit of detection and the limit of quantification for indacaterol and mometasone were 0.03 and 0.10 μg mL-1 while for glycopyrronium, they were 0.16 and 0.50 μg mL-1.</p><p><strong>Highlights: </strong></p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10139259","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 Sensitive Liquid Chromatography-Mass Spectrometric Method for Determination of Bisoprolol in Rat Serum after Pre-Column Derivatization. 柱前衍生化后测定大鼠血清中比索洛尔的灵敏液相色谱-质谱法
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmad056
Huda A Shaheen, Saleh O Bahaffi, Alaa M Khedr
{"title":"A Sensitive Liquid Chromatography-Mass Spectrometric Method for Determination of Bisoprolol in Rat Serum after Pre-Column Derivatization.","authors":"Huda A Shaheen, Saleh O Bahaffi, Alaa M Khedr","doi":"10.1093/chromsci/bmad056","DOIUrl":"10.1093/chromsci/bmad056","url":null,"abstract":"<p><p>Two derivatization regents were reacted with bisoprolol (BIS), followed by liquid-chromatography-mass spectrometric analysis. 3-Bromomethyl-propyphenazone (BMP) and dansyl-chloride (Dns-Cl) were reacted via the secondary amino group using a catalyst to accelerate the reaction progress and completeness with minimal reaction byproducts. The sensitivity and the ionization efficiency of both BIS-methyl-propyphenazone (BIS-MP) and BIS-Dns via electrospray ionization were studied. The sensitivity of BIS-MP was superior to BIS-Dns. The derivatization procedure, extraction procedure, and LC-MS method were optimized and validated to achieve the monitoring of BIS in rat serum at a picogram scale. The calibration curve showed a regression coefficient value of 0.999 within a concentration spanning a range of 10-500 pg/mL. The detection limit and quantitation were 4 and 10 pg/mL, respectively. The intraday and inter-day precision values (% relative standard deviation) ranged from 0.53 to 6.91%, whereas the accuracy values (expressed as % error) ranged from -4.20 to -0.77%. The pharmacokinetic parameters were: 15,280 pg/mL for a maximum concentration of BIS (Cmax) at the maximum time (Tmax) of 1 h. BIS's elimination half-life (t1/2) was determined to be 3 h. The value of the area under the concentration-time curve (AUC0 - t) was 34,370 pg/mL h.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9890505","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
LC and LC-MS/MS Studies for the Separation and Identification of Impurities and Degradation Products of Betaxolol. 用于分离和鉴定倍他洛尔杂质和降解产物的 LC 和 LC-MS/MS 研究。
IF 1.5 4区 化学
Journal of chromatographic science Pub Date : 2024-08-20 DOI: 10.1093/chromsci/bmae025
Anis Chmangui, Mehdi Safta, Mohamed Ridha Driss, Soufiane Touil, Sondes Bouabdallah
{"title":"LC and LC-MS/MS Studies for the Separation and Identification of Impurities and Degradation Products of Betaxolol.","authors":"Anis Chmangui, Mehdi Safta, Mohamed Ridha Driss, Soufiane Touil, Sondes Bouabdallah","doi":"10.1093/chromsci/bmae025","DOIUrl":"10.1093/chromsci/bmae025","url":null,"abstract":"<p><p>Betaxolol (Bx) is a selective β1 receptor blocker used in the treatment of hypertension and glaucoma. The aim of the present work was to demonstrate an approach involving use of liquid chromatography (LC) and liquid chromatography-electrospray ionization mass spectrometry (LC-ESI/MS) for the simultaneous separation, identification and characterization of impurities and of degradation products of betaxolol without their isolation from the reaction mixtures. At optimum condition, and according to ICH guidelines, the limit of detection (LOD) and limit of quantification (LOQ) for Bx are found to be 5.46 and 16.54 μg mL-1, respectively. However, the LOD and LOQ for the major degradation product P6 were 2.15 and 6.53 μg mL-1. Betaxolol was subjected to hydrolytic (acidic and basic) and oxidative, stress conditions according to International Conference on Harmonization (ICH) guideline Q1A (R2), and as results, the drug was found to be labile in acidic, basic and oxidative stress conditions. Based on LC-ESI/MS analysis, the found results revealed that Bx decomposes in acidic, basic and oxidizing environments. All degradation products were identified with the help of their fragmentation pattern and the masses obtained upon the MS analysis.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140876569","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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