{"title":"Stability Indicating Method Development and Validation of Glycyrrhizin Using RP-HPLC-DAD: Application to Glycyrrhiza glabra Extract.","authors":"Waibiangki Lyngdoh, Sandeep Jat, Pramod Kumar","doi":"10.1093/chromsci/bmae022","DOIUrl":"10.1093/chromsci/bmae022","url":null,"abstract":"<p><p>Glycyrrhiza glabra is commonly known as licorice. Licorice is the major source of glycyrrhizin. There is no reported stability indicating method for glycyrrhizin in the literature so far. Therefore, it was proposed to develop a stability indicating method and validate the method for glycyrrhizin and its application in G. glabra root extract. Method validation parameters were performed as per the International Council for Harmonization guidelines. The chromatographic separation was achieved on a Zorbax Extended C-18 (250 × 4.6 mm, 5 μm) column. The separation achieved using the mobile phase consisted of 0.1% formic acid in water and acetonitrile in gradient elution. The flow rate was kept at 1 mL/min, and ultraviolet-visible spectroscopy detection was at 250 nm. The average retention time of glycyrrhizin was found to be 7.30 min. Stress degradation studies were performed and confirmed that only acidic degradation has shown a degradation profile of glycyrrhizin up to 40%. The percentage of glycyrrhizin was found to be 0.40% in the G. glabra extract. This may be further explored for commercial applications.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140849307","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":"Chromatographic Separation and Quantification of Nine Nitrosamine Genotoxic Impurities in a Single Method in Nebivolol Tablet by Using Validated Ultra-Sensitive Liquid Chromatography: Mass Spectrometry Analytical Method.","authors":"Mehul Pathak, Dhara D Patel, Dalip Kumar, Avineesh Singh, Suresh Agrawal","doi":"10.1093/chromsci/bmae061","DOIUrl":"10.1093/chromsci/bmae061","url":null,"abstract":"<p><p>N-nitrosamine impurities have been detected in a vast variety of drug substances and drug products, showing concern for regulatory aspects. To meet the regulatory requirement for the concerned impurity, a sensitive analytical method capable of quantifying these impurities at a lower level with accuracy and precision is required. This article focuses on the development and validation of an analytical method for the simultaneous detection of nine nitrosamine impurities in a single method for nebivolol drug product using liquid chromatography-mass spectrometry/mass spectrometry-atmospheric pressure chemical ionization (LC-MS/MS-APCI). The chromatographic separation was performed using the LC-MS column Allure BiPh C18 (250 × 4.6 mm), 5 μm employed a gradient mode elution program using 0.002 M Ammonium acetate buffer pH 4.5 as mobile phase A and methanol as mobile phase B. The method was challenged for accuracy, precision and linearity in accordance with International Council for Harmonization guidelines to ensure its suitability for the intended usage. The developed method was specific, accurate and linear with square of correlation coefficient (r2) found to be greater than 0.99 (0.9970-0.9992). The LOQ obtained in the range of 9.85-19.62 ppb for nine nitrosamines showed good sensitivity. The results demonstrated that method can be applied to quantify the nitrosamines in nebivolol drug products.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142894941","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":"Using the AQbD Approach, Development and Validation of a Simple, Rapid Stability Indicating Chromatographic Method for Quantification of Related Impurities of Apixaban.","authors":"Jayasri Kilari, Pradeep Kumar Brahman","doi":"10.1093/chromsci/bmad065","DOIUrl":"10.1093/chromsci/bmad065","url":null,"abstract":"<p><p>Apixaban is a new oral anticoagulant that has been approved by the United States Food and Drug Administration for the prevention of stroke and other cardiovascular complications in people with non-valvular atrial fibrillation. Then, later, it was given the green light to treat deep venous thrombosis and pulmonary embolism. The biggest challenge in the development of pharmaceutical drugs is comprehending science- and risk-based techniques for developing and maintaining analytical procedures appropriate for evaluating the quality of drug substances and drug products. The improved technique provides a methodical strategy to acquire and improve understanding of an analytical method. The current study discusses the related substances method development for an apixaban drug substance employing a regulated authority refined and approved approach of the quality-by-design concept. For the quantification of impurities, and apixaban drug substance, a simple, quick and stability-indicating reverse-phase liquid chromatographic method was developed using a full factorial design. The separation between apixaban and its nine impurities was accomplished using an Zorbax Stable Bond Phenyl, 150 × 4.6 mm, 5 μm column. The mobile-phase components for gradient elution at a flow rate of 1.2 mL/min were chosen to be a mixture of water, acetonitrile, methanol and perchloric acid in various ratios with a total run time of 15 min. Chromatograms were extracted at 278 nm after a 5 μL solution injection. According to regulatory requirements, the developed method has been validated for its intended purpose.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"978-989"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10018713","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":"Comparison of Plasma Concentration of Linezolid's Detection by FICA and LC-MS/MS.","authors":"Jing Chen, Chenxia Zhu, Yangjin He, Hengbin Cao","doi":"10.1093/chromsci/bmae003","DOIUrl":"10.1093/chromsci/bmae003","url":null,"abstract":"<p><p>Linezolid was the first totally synthetic oxazolidinone antibiotic that was approved for clinical use against Mycobacterium tuberculosis. Our study investigated the correlation and consistency of fluorescence immunochromatography assay (FICA) and high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) in measuring linezolid levels in the plasma. Plasma samples were collected from 80 to 100 tuberculosis patients. The samples were analyzed by FICA and LC-MS/MS, and linezolid levels measured by the two methods were compared by outlier test, correlation coefficient, Bland-Altman scatter plot, Deming regression analysis and bias evaluation. A total of 83 plasma samples were collected, all of which were non-outlier. The correlation coefficient of FICA and LC-MS/MS results was 0.9845. Deming regression analysis showed that the regression equation of FICA and LC-MS/MS was y = 0.2229 + 1.0076x. The medical decision levels of 2 and 7 μg/mL were taken into the regression equation, and the 95% CI of 2- and 7-μg/mL bias were both within the allowed error range. The findings indicated a strong correlation between the results obtained from FICA and LC-MS/MS were consistent showed good correlation, demonstrating their equivalence in measurement.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"990-994"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139746734","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":"Nanoparticle Assisted Fabric Phase Sorptive Extraction for Azo Dye Determination in the Industrial Sewage.","authors":"Nayereh Rahimian, Javad Feizy, Zarrin Es'haghi","doi":"10.1093/chromsci/bmae046","DOIUrl":"10.1093/chromsci/bmae046","url":null,"abstract":"<p><p>Currently, one of the significant environmental problems is the presence of azo dye materials in water sources. In this study, for the first time, a fast and sensitive sample preparation approach using nanoparticle-assisted fabric phase sorptive extraction (NFPSE) followed by high-performance liquid chromatography was examined to remove some azo dyes such as methyl red and sunset yellow from aqueous solutions. Primarily, the significance of several parameters affecting NFPSE, such as fabric type, the kind of sorbent, the number of contacts with sol-gel and the time of contact, was investigated. In addition, experiments were performed to determine the effect of different adsorption parameters, such as sample volume, adsorption time, adsorbent value, desorption time, ionic strength and pH. It was found that the calibration curve was linear within two ranges of concentrations (0.05-0.1 and 0.5-15 ng/L for methyl red; 0.05-0.5 and 0.5-15 ng/L for sunset yellow) with correlation coefficients better than 0.9683. The limit of detection was 0.014 ng/L for methyl red and 0.015 ng/L for sunset yellow. Repeatability Relative Standard Deviation (RSD) with three replicated experiments was 1.5-10% for methyl red and 2.5-5.8% for sunset yellow. Relative recovery percentages of 88-96% for methyl red and 62-92% for sunset yellow were obtained in the samples. Moreover, the results have shown that acceptable accuracy, precision and linearity make the \"fabric phase sorptive extraction\" a proper method for the determination of dyes from industrial sewage samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"995-1006"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141893545","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":"A Novel Method for Determination of Cyclobenzaprine in the Different Matrixes by UHPLC-DAD: Application to Real Human Plasma and Pharmaceutical Formulations.","authors":"Tugrul C Akman","doi":"10.1093/chromsci/bmad052","DOIUrl":"10.1093/chromsci/bmad052","url":null,"abstract":"<p><p>This study presents a novel and efficient method for determining of cyclobenzaprine (CBP) in human plasma and tablets using simple liquid-liquid microextraction and ultra-high performance liquid chromatography-diode-array detector. The developed method was optimized and validated for selectivity, linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). The chromatographic separation was achieved using a C18 column with a mobile phase consisting of a mixture of deionized water containing 0.1% TFA and methanol (30:70, v:v) at a flow rate of 1.0 mL/min. The extraction process provided high-efficiency recovery of CBP with a small plasma volume (%94.3). The method showed good linearity within the concentration range of 0.005-10 μg/mL, with a correlation coefficient of 0.999. The LOD and LOQ values were found to be 0.0013 and 0.005 μg/mL, respectively. The intra- and inter-day %RSD were <8%, and %RE were ranged from -0.50 to 0.01%. The proposed method was successfully applied to the analysis of CBP in real human plasma samples and tablets, indicating its applicability in clinical and pharmaceutical research. In conclusion, the simple, low cost, high sensitivity and rapid nature of this method make it an attractive option for the quantification of CBP in human plasma and pharmaceutical dosage forms.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"953-961"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9890502","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":"Implementation of White Analytical Chemistry-Assisted Analytical Quality by Design Approach to Green Liquid Chromatographic Method for Concomitant Analysis of Anti-Hypertensive Drugs in Human Plasma.","authors":"Pintu Prajapati, Abhinandan Shahi, Aneri Acharya, Veera Shakar Pulusu, Shailesh Shah","doi":"10.1093/chromsci/bmad054","DOIUrl":"10.1093/chromsci/bmad054","url":null,"abstract":"<p><p>According to current concepts of white analytical chemistry (WAC), the use of organic solvents those are teratogenic and carcinogenic must be avoided for the protection of the environment and of the analysts. This led to the development and validation of the WAC-assisted green liquid chromatographic technique (reverse-phase high-pressure liquid chromatography (RP-HPLC)) for the simultaneous analysis of anti-hypertensive drugs (azilsartan medoxomil, chlorthalidone and cilnidipine) in human plasma and their fixed-dose combinations. The analytical quality by design approach was used in conjunction with the design of experiments and chemometrics concepts to develop the method. To develop the green RP-HPLC method, critical method variables (CMVs) and critical analytical attributes were identified using the multivariate analytical tools principal component analysis and partial least square regression. Using the Box-Behnken design, the design of experiments was used for CMV optimization and response surface analysis. It was possible to explore the analytical design space for the life cycle management of the RP-HPLC method. The developed method was found to be validated following International Council for Harmonization Q2 (R1) and M10 requirements. Using the red, green and blue paradigm, the existing and proposed chromatographic methods were evaluated for their validation efficacy, greenness profile and cost-effectiveness.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"938-952"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10268978","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}
Chaoqun Chang, Xinghua Jin, Hui Bai, Fan Zhang, Lei Chen
{"title":"Molecular Dynamics Simulation for the Acidic Compounds Retention Mechanism Study on Octyl-Quaternary Ammonium Mixed-Mode Stationary Phase.","authors":"Chaoqun Chang, Xinghua Jin, Hui Bai, Fan Zhang, Lei Chen","doi":"10.1093/chromsci/bmae036","DOIUrl":"10.1093/chromsci/bmae036","url":null,"abstract":"<p><p>With the widespread application of mixed-mode chromatography in separation analysis, it is becoming increasingly important to study its retention mechanism. The retention behavior of acidic compounds on mixed-mode octyl-quaternary ammonium (Sil-C8-QA) columns was investigated by computer simulation. Firstly, the benzoic acid homologues were used as the analytes, and the simulation model was constructed by the Materials Studio. Geometric optimization, annealing and molecular dynamics (MD) simulation of these complexes resulted in optimized conformations. The binding energy, mean square displacement (MSD) and torsion angle distribution generated by MD simulation were then analyzed. The results showed that the more negative binding energy, the greater the MSD and the narrower the torsion angle distribution, indicating that the stationary phase behaves with stronger interaction and retention. The retention behavior of five acidic drugs on the Sil-C8-QA column was then successfully explained by simulation. Acidic drugs are more retentive on the mixed-mode column due to the more substantial interaction brought by the reversed-phase/ion-exchange mixed-mode mechanism compared to other single-mode columns. This simulation method is expected to provide ideas for studying the separation mechanism and predicting the retention behavior of more complex samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"962-971"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141158330","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}
Chandramauly R Sharma, Vijay Mishra, Yadvendra Agrawal
{"title":"RP-HPLC Study of the Complexation of Acetamiprid, Imidacloprid and Carboxin Guest Molecules With Thiophosphorylated Calix [6] Arene in Dimethylformamide-Acetonitrile-Water Mobile Phase.","authors":"Chandramauly R Sharma, Vijay Mishra, Yadvendra Agrawal","doi":"10.1093/chromsci/bmae052","DOIUrl":"10.1093/chromsci/bmae052","url":null,"abstract":"<p><p>Reversed-phase high-performance liquid chromatography was used to study the host-guest complexation of thiophosphacalixarenes (TPC 1-3) with acetamiprid, imidacloprid and carboxin as guests. The Onyx Monolithic C 18 column (150 × 0.1 mm) and Phenomenex® were used with UV detection at 254 nm. The mobile phase consisted of dimethylformamide-acetonitrile-water. The association constant of the 1:1 guest-host complexes was determined from the relationship between the retention factor of the guest and concentration of the thiophosphacalix [6] arene host in the mobile phase. The stability constants are influenced by size, nature, position and quantity of substituents in the benzene ring of the calixarene skeleton. The detection limits for TPC 1, TPC 2 and TPC 3 are 0.95, 1.20 and 1.40 μg/mL, while the quantification limits are 2.85, 3.60 and 4.20 μg/mL for TPC 1, TPC 2 and TPC 3, respectively.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"972-977"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142390924","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 Residual Dimethyl Sulfate in Cephalosporin Using HS-SPME/GC-MS.","authors":"Rongchun Lu","doi":"10.1093/chromsci/bmae054","DOIUrl":"10.1093/chromsci/bmae054","url":null,"abstract":"<p><p>Dimethyl sulfate (DMS) is widely used in manufacturing process but because of its genotoxicity nature, it should be monitored at trace levels (1 μg/mL). It is complicated and difficult to quantify DMS in cephalosporin with traditional method. Herein, a method for quantifying residual DMS in cephalosporin was developed, without complex sample preprocessing, no need for a large amount of solvent, employing headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS). Compared with polydimethylsiloxane (PDMS)/divinylbenzene and polyacrylate fibers, PDMS was more suitable for absorbing DMS. The research showed that the PDMS fiber should be changed after 50 adsorption-desorption cycles. Linear regression analysis of the calibration curve demonstrated a robust linear relationship, with R2 of 0.999, across a concentration range of 0.25 to 4.0 μg/mL. The method underwent rigorous validation for specificity, linearity, precision and accuracy. This method was proven effective in measuring DMS in complex matrices. The limits of detection and quantification for this method is 0.05 and 0.25 μg/mL, respectively, which has room for improvement.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"922-928"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142501225","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}