A. Gören, Betül Kiraz Kinoğlu, T. Dirmenci, Saleh H. Alwasel, I. Gülçin
{"title":"Quantification of main secondary metabolites of Satureja icarica P.H. Davis (Lamiaceae) by LC-HRMS and evaluation of antioxidant capacities","authors":"A. Gören, Betül Kiraz Kinoğlu, T. Dirmenci, Saleh H. Alwasel, I. Gülçin","doi":"10.25135/jcm.2311.2956","DOIUrl":"https://doi.org/10.25135/jcm.2311.2956","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138971592","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-14DOI: 10.25135/jcm.98.2311.2975
Rajesh Varma Bhupatiraju, B. S. Kumar, Pavani Peddi, V. Tangeti
{"title":"An effective HPLC method for evaluation of process related impurities of Letermovir and LC-MS/MS characterization of forced degradation compounds","authors":"Rajesh Varma Bhupatiraju, B. S. Kumar, Pavani Peddi, V. Tangeti","doi":"10.25135/jcm.98.2311.2975","DOIUrl":"https://doi.org/10.25135/jcm.98.2311.2975","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138974645","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-11-30DOI: 10.25135/jcm.97.2307.2859
O. Pınarbaşlı, Tolga Özbay, G. Gurbetoğlu, Nagehan Sarraçoğlu, Asuman Aybey Doganay
: This study aimed to establish and validate a reliable RP-HPLC assay method for the quantification of tofacitinib (TFC), a janus kinase (JAK) inhibitor, in pharmaceutical formulations. The newly developed method exhibits simplicity, specificity, precision, and sensitivity. Experimental procedures utilized a Shimadzu Prominence 20A HPLC system equipped with a Inertsil ODS 3V C18 column (5µm particle size, 4.6 X 250 mm dimensions). The mobile phase, consisting of 0.05M ammonium acetate buffer at pH 5.0 and acetonitrile (65:35 v/v) in isocratic mode with a flow rate of 1.0 mL/min, facilitated accurate detection of the Tofacitinib peak at 230 nm wavelength. Comprehensive validation, including assessments of linearity, accuracy, precision, and robustness, was conducted in accordance with ICH requirements. The results demonstrated satisfaction, with a retention time (t R ) of approximately 5.3 minutes. The imperative need for a swift and efficient RP-HPLC method for analyzing TFC led to the successful development and validation of this technique. Consequently, the RP-HPLC method has undergone thorough validation, establishing it as a user-friendly and trustworthy means for Tofacitinib analysis.
:本研究旨在建立并验证一种可靠的RP-HPLC检测方法，用于定量检测药物制剂中的破伤风激酶（JAK）抑制剂托法替尼（TFC）。新开发的方法简便、特异、精确、灵敏。实验采用岛津Prominence 20A高效液相色谱仪，配备Inertsil ODS 3V C18色谱柱（5µm粒径，4.6 X 250 mm）。流动相由 pH 值为 5.0 的 0.05M 醋酸铵缓冲液和乙腈（65:35 v/v）组成，采用等度模式，流速为 1.0 mL/min，有助于在 230 nm 波长处准确检测托法替尼峰。根据 ICH 要求进行了全面验证，包括线性、准确度、精密度和稳健性评估。结果表明，保留时间（t R ）约为 5.3 分钟，令人满意。由于迫切需要一种快速高效的 RP-HPLC 方法来分析 TFC，因此成功开发并验证了这一技术。因此，RP-HPLC 方法经过了全面的验证，使其成为分析托法替尼的一种便于使用且值得信赖的方法。
{"title":"A validated RP-HPLC assay method for Tofacitinib in pharmaceutical drug products","authors":"O. Pınarbaşlı, Tolga Özbay, G. Gurbetoğlu, Nagehan Sarraçoğlu, Asuman Aybey Doganay","doi":"10.25135/jcm.97.2307.2859","DOIUrl":"https://doi.org/10.25135/jcm.97.2307.2859","url":null,"abstract":": This study aimed to establish and validate a reliable RP-HPLC assay method for the quantification of tofacitinib (TFC), a janus kinase (JAK) inhibitor, in pharmaceutical formulations. The newly developed method exhibits simplicity, specificity, precision, and sensitivity. Experimental procedures utilized a Shimadzu Prominence 20A HPLC system equipped with a Inertsil ODS 3V C18 column (5µm particle size, 4.6 X 250 mm dimensions). The mobile phase, consisting of 0.05M ammonium acetate buffer at pH 5.0 and acetonitrile (65:35 v/v) in isocratic mode with a flow rate of 1.0 mL/min, facilitated accurate detection of the Tofacitinib peak at 230 nm wavelength. Comprehensive validation, including assessments of linearity, accuracy, precision, and robustness, was conducted in accordance with ICH requirements. The results demonstrated satisfaction, with a retention time (t R ) of approximately 5.3 minutes. The imperative need for a swift and efficient RP-HPLC method for analyzing TFC led to the successful development and validation of this technique. Consequently, the RP-HPLC method has undergone thorough validation, establishing it as a user-friendly and trustworthy means for Tofacitinib analysis.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-11-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139197705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-11-09DOI: 10.25135/jcm.95.2308.2862
Mustafa Özyürek, Mehmet Kılınçer
: Measurement uncertainty is a metrological concept that characterizes distributions/variations that can make the measurement results logical and is linked to the result of the measurement. The measurement uncertainty of the method was estimated using two basic approaches (top-down and bottom-up approach). The top-down approach covers in-house validation data (trueness, repeatability and intra-lab reproducibility), while the bottom-up approach involves individual contributions to all uncertainty at each stage of the analysis/process. We estimated measurement uncertainty of BPA analysis by HPLC-FLD test according to JCGM GUM and EURACHEM-CITAC guidelines. The relative expanded uncertainties at the BPA concentration by the bottom-up approach and top-down approaches were ±3.2% and ±4.8% respectively (95% confidence interval, k=2). Thus, although it is seen that the results of the two approaches are different in chromatographic BPA analysis, it is concluded that the measurement uncertainty related to BPA analysis, especially in food analysis laboratories, can be determined by a simpler top-down approach.
{"title":"Comparison between top-down and bottom-up approaches in the estimation of measurement uncertainty in Bisphenol A analysis by HPLC-FLD","authors":"Mustafa Özyürek, Mehmet Kılınçer","doi":"10.25135/jcm.95.2308.2862","DOIUrl":"https://doi.org/10.25135/jcm.95.2308.2862","url":null,"abstract":": Measurement uncertainty is a metrological concept that characterizes distributions/variations that can make the measurement results logical and is linked to the result of the measurement. The measurement uncertainty of the method was estimated using two basic approaches (top-down and bottom-up approach). The top-down approach covers in-house validation data (trueness, repeatability and intra-lab reproducibility), while the bottom-up approach involves individual contributions to all uncertainty at each stage of the analysis/process. We estimated measurement uncertainty of BPA analysis by HPLC-FLD test according to JCGM GUM and EURACHEM-CITAC guidelines. The relative expanded uncertainties at the BPA concentration by the bottom-up approach and top-down approaches were ±3.2% and ±4.8% respectively (95% confidence interval, k=2). Thus, although it is seen that the results of the two approaches are different in chromatographic BPA analysis, it is concluded that the measurement uncertainty related to BPA analysis, especially in food analysis laboratories, can be determined by a simpler top-down approach.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135286422","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Development and validation of RP-HPLC method for estimation of Torsemide and Spironolactone in bulk and pharmaceutical dosage forms: a quality by design approach","authors":"Tejas Patel, Shantilal Padhiyar, Vipul Prajapati, Harsh Kela, Vashisth Bhavsar, Jagat Upadhyay","doi":"10.25135/jcm.94.2304.2769","DOIUrl":"https://doi.org/10.25135/jcm.94.2304.2769","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135724983","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
: Simple, accurate, precise, and sensitive reverse-phase high-performance liquid chromatographic (HPLC) method was developed for the simultaneous measurement of ARI and ESC in pharmaceutical products by using a C18 column with dimensions of 250 mm x 4.6 mm and a particle size of 5 μm. The mobile phase consisted of a mixture of acetonitrile, methanol, and water in the ratio of 80:05:15 v/v/v. Orthophosphoric acid was added to adjust the pH to 7.00 ± 0.1. The detection wavelength used for measuring the absorbance of the components was 246 nm, and the Mobile Phase flow rate was set at 1.0 mL/min. The retention times of ARI and ESC were 5.63 and 3.65 minutes, respectively. The ARI and ESC correlation coefficients (R 2 -values) were observed at 0.9995 and 0.9997, respectively, demonstrating a robust linear relationship between the analyte concentration and the observed absorbance. The linearity range for ARI was 20 to 120 μg/mL, while ESC was 60 to 360 μg/mL. The recovery percentages for ARI and ESC ranged from 99.43% to 100.65% and 99.58% to 100.15%, respectively. Additionally, all parameter uncertainty levels were below 2. The method was validated following ICH guideline Q2 (R1). The analytical method validated will be successfully applied to the pharmaceutical dosage form.
{"title":"Simultaneous determiantion of aripiprazole and escitalopram oxalate by HPLC","authors":"Divyakumari Kiransinh Solanki, Sagarkumar P. Patel, Jasmina Surati, Ashok Akabari, Ketan Shah, Dipansu Sahu, Sagarkumar Patel","doi":"10.25135/jcm.92.2307.2830","DOIUrl":"https://doi.org/10.25135/jcm.92.2307.2830","url":null,"abstract":": Simple, accurate, precise, and sensitive reverse-phase high-performance liquid chromatographic (HPLC) method was developed for the simultaneous measurement of ARI and ESC in pharmaceutical products by using a C18 column with dimensions of 250 mm x 4.6 mm and a particle size of 5 μm. The mobile phase consisted of a mixture of acetonitrile, methanol, and water in the ratio of 80:05:15 v/v/v. Orthophosphoric acid was added to adjust the pH to 7.00 ± 0.1. The detection wavelength used for measuring the absorbance of the components was 246 nm, and the Mobile Phase flow rate was set at 1.0 mL/min. The retention times of ARI and ESC were 5.63 and 3.65 minutes, respectively. The ARI and ESC correlation coefficients (R 2 -values) were observed at 0.9995 and 0.9997, respectively, demonstrating a robust linear relationship between the analyte concentration and the observed absorbance. The linearity range for ARI was 20 to 120 μg/mL, while ESC was 60 to 360 μg/mL. The recovery percentages for ARI and ESC ranged from 99.43% to 100.65% and 99.58% to 100.15%, respectively. Additionally, all parameter uncertainty levels were below 2. The method was validated following ICH guideline Q2 (R1). The analytical method validated will be successfully applied to the pharmaceutical dosage form.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136294936","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-09-04DOI: 10.25135/jcm.91.2307.2837
Cem Çalışkan, Onur Çakır, Muge Guleli, Yavuz Selim Toksöz, H. I. Uğraş
: For sachet drug forms containing Racecadotril, which are freely soluble in methanol and methylene chloride but practically insoluble in water, used as an anti-diarrhea, suitable dissolution media meeting the parameters requested by the authorities are not available in the literature and monographs. For this reason, a suitable dissolution medium was determined in accordance with the guidelines and the dissolution profiles of reference product and samples used in the study. The profiles were compared, and the method was validated. In order to determine the most suitable medium for the release of drug product, in vitro dissolution tests were performed in media prepared by different buffers similar to the pH of the gastrointestinal tract (GIT) and media containing Brij 35. In this context, the effects of buffers, pH, and different surfactants were evaluated, and it was found that Polyoxyethylene 23 lauryl ether (Brij-35), a nonionic surfactant, increased the solubility. The results were obtained with RP-HPLC method using Kromasil C18 150 mm x 4.6 mm, 5 µm column with a flow rate of 1.5 ml/min at 210 nm wavelength in 7 minutes for Racecadotril, which dissolves at least 60% of the label value after 45 minutes after the dissolution studies performed with a type II apparatus at 37°C. A suitable dissolution medium was found for sachet drug forms containing Racecadotril, and the analytical method was validated in accordance with the ICH Q2 (R1) guideline. In addition, the difference factor (f 1 ) and similarity factor (f 2 ) were calculated to compare the dissolution profiles of the reference product and samples in this determined dissolution medium.
：对于含有Racecadotril的小袋剂型，其可自由溶于甲醇和二氯甲烷，但实际上不溶于水，用作止泻剂，文献和专著中没有符合当局要求参数的合适溶解介质。因此，根据研究中使用的参考产品和样品的指南和溶解特性，确定了合适的溶解介质。对这些剖面进行了比较，并对该方法进行了验证。为了确定最适合释放药物产品的培养基，在由类似胃肠道（GIT）pH的不同缓冲液制备的培养基和含有Brij 35的培养基中进行体外溶出试验。在这种情况下，评估了缓冲液、pH和不同表面活性剂的影响，发现非离子表面活性剂聚氧乙烯23十二烷基醚（Brij-35）增加了溶解度。结果通过RP-HPLC法获得，使用Kromasil C18 150 mm x 4.6 mm，5µm柱，流速为1.5 ml/min，波长为210 nm，用于Racecadotril，在37°C下用II型仪器进行溶解研究后，45分钟后溶解至少60%的标记值。为含有Racecadotril的小袋剂型找到了合适的溶出介质，并根据ICH Q2（R1）指南验证了分析方法。此外，还计算了差异因子（f1）和相似因子（f2），以比较参考产品和样品在该确定的溶解介质中的溶解特性。
{"title":"In-vitro release study of Racecadotril from granule sachets: influence of Brij-35","authors":"Cem Çalışkan, Onur Çakır, Muge Guleli, Yavuz Selim Toksöz, H. I. Uğraş","doi":"10.25135/jcm.91.2307.2837","DOIUrl":"https://doi.org/10.25135/jcm.91.2307.2837","url":null,"abstract":": For sachet drug forms containing Racecadotril, which are freely soluble in methanol and methylene chloride but practically insoluble in water, used as an anti-diarrhea, suitable dissolution media meeting the parameters requested by the authorities are not available in the literature and monographs. For this reason, a suitable dissolution medium was determined in accordance with the guidelines and the dissolution profiles of reference product and samples used in the study. The profiles were compared, and the method was validated. In order to determine the most suitable medium for the release of drug product, in vitro dissolution tests were performed in media prepared by different buffers similar to the pH of the gastrointestinal tract (GIT) and media containing Brij 35. In this context, the effects of buffers, pH, and different surfactants were evaluated, and it was found that Polyoxyethylene 23 lauryl ether (Brij-35), a nonionic surfactant, increased the solubility. The results were obtained with RP-HPLC method using Kromasil C18 150 mm x 4.6 mm, 5 µm column with a flow rate of 1.5 ml/min at 210 nm wavelength in 7 minutes for Racecadotril, which dissolves at least 60% of the label value after 45 minutes after the dissolution studies performed with a type II apparatus at 37°C. A suitable dissolution medium was found for sachet drug forms containing Racecadotril, and the analytical method was validated in accordance with the ICH Q2 (R1) guideline. In addition, the difference factor (f 1 ) and similarity factor (f 2 ) were calculated to compare the dissolution profiles of the reference product and samples in this determined dissolution medium.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48408583","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-29DOI: 10.25135/jcm.88.2304.2753
Shrikant Shivaji Pawade, Ivo Leito, Koit Herodes, Lauri Toom
{"title":"Accuracy of quantitative NMR analysis: a case study of lignin","authors":"Shrikant Shivaji Pawade, Ivo Leito, Koit Herodes, Lauri Toom","doi":"10.25135/jcm.88.2304.2753","DOIUrl":"https://doi.org/10.25135/jcm.88.2304.2753","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134999380","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-29DOI: 10.25135/jcm.87.2303.2773
Adel Shehata, Abdulrahman R. Alaskar, Rashed A. Aldosari, Fahad R. Almutairi
{"title":"Certification of buffer solutions reference materials using Baucke cell for supporting the quality of pH measurements","authors":"Adel Shehata, Abdulrahman R. Alaskar, Rashed A. Aldosari, Fahad R. Almutairi","doi":"10.25135/jcm.87.2303.2773","DOIUrl":"https://doi.org/10.25135/jcm.87.2303.2773","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134999378","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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