{"title":"Development of a stability-indicating HPLC method for Lasmiditan and its process related impurities with characterization of degradation products by LCMS/MS","authors":"Venkateswara Rao Anna, Chilakabattina Naga Narasimha Babu, Bhagya Kumar Tatavarti, N. Vijaya, Cherukula Srinivasa Reddy","doi":"10.25135/jcm.89.2304.2767","DOIUrl":"https://doi.org/10.25135/jcm.89.2304.2767","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45206877","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.90.2304.2599
A. Gören, T. Akalin, S. Yalçin, Aysenur Gunaydin Akyildiz
{"title":"Determination of adulteration in hair serums by LC-HRMS §","authors":"A. Gören, T. Akalin, S. Yalçin, Aysenur Gunaydin Akyildiz","doi":"10.25135/jcm.90.2304.2599","DOIUrl":"https://doi.org/10.25135/jcm.90.2304.2599","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46687070","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/rnp.84.2212.2661
Shantilal Padhiyar, Kamlesh M Jivani, J. Upadhyay, Tejas Patel, V. Bhavsar, B. Suhagia
{"title":"Chemometrics assisted UV-spectrophotometric method for simultaneous estimation of aliskiren and hydrochlorothiazide in bulk and their pharmaceutical dosage form","authors":"Shantilal Padhiyar, Kamlesh M Jivani, J. Upadhyay, Tejas Patel, V. Bhavsar, B. Suhagia","doi":"10.25135/rnp.84.2212.2661","DOIUrl":"https://doi.org/10.25135/rnp.84.2212.2661","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-06-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45467834","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 : 2023-05-19DOI: 10.25135/rnp.87.2303.2773
A. Shehata, A. R. Alaskar, Rashed A. Aldosari, F. Almutairi
: The need for certified pH reference materials to support the traceability claims and quality of the daily large volume of pH measurements is very strong. In this work, three batches of buffer solutions were prepared, and their pH values were certified in accordance with the IUPAC Recommendation 2002. The first batch was prepared from potassium tetraoxalate (dihydrate) and disodium oxalate to provide pH4 and the second batch was prepared from disodium hydrogen phosphate and potassium dihydrogen phosphate to provide pH7. The third batch was prepared from sodium hydrogen carbonate and sodium carbonate to provide pH10. Every batch was homogenized by mechanical shaking for one night and bottled into 50 HDPE bottles, each is 250 mL. A number of bottles were systematically selected for homogeneity, stability and characterization studies of the buffer reference materials. These studies were carried out in accordance with the requirements of ISO 17034 and ISO Guide 35 using Baucke cell. The pH values 4, 7 and 10 of the secondary buffers were restandardized with regard to the pH values 4, 7 and 10 of the primary buffers produced by the Slovak National Metrology Institute, SMU. The results obtained showed that the produced buffer RMs were homogeneous and stable enough and their certified pH values were found 4.001±0.019, 7.005±0.015 and 10.002±0.023. These CRMs will be very useful as calibrants and as PT samples for analytical laboratories performing pH measurements in various fields.
{"title":"Certification of buffer solutions reference materials using Baucke cell for supporting the quality of pH measurements","authors":"A. Shehata, A. R. Alaskar, Rashed A. Aldosari, F. Almutairi","doi":"10.25135/rnp.87.2303.2773","DOIUrl":"https://doi.org/10.25135/rnp.87.2303.2773","url":null,"abstract":": The need for certified pH reference materials to support the traceability claims and quality of the daily large volume of pH measurements is very strong. In this work, three batches of buffer solutions were prepared, and their pH values were certified in accordance with the IUPAC Recommendation 2002. The first batch was prepared from potassium tetraoxalate (dihydrate) and disodium oxalate to provide pH4 and the second batch was prepared from disodium hydrogen phosphate and potassium dihydrogen phosphate to provide pH7. The third batch was prepared from sodium hydrogen carbonate and sodium carbonate to provide pH10. Every batch was homogenized by mechanical shaking for one night and bottled into 50 HDPE bottles, each is 250 mL. A number of bottles were systematically selected for homogeneity, stability and characterization studies of the buffer reference materials. These studies were carried out in accordance with the requirements of ISO 17034 and ISO Guide 35 using Baucke cell. The pH values 4, 7 and 10 of the secondary buffers were restandardized with regard to the pH values 4, 7 and 10 of the primary buffers produced by the Slovak National Metrology Institute, SMU. The results obtained showed that the produced buffer RMs were homogeneous and stable enough and their certified pH values were found 4.001±0.019, 7.005±0.015 and 10.002±0.023. These CRMs will be very useful as calibrants and as PT samples for analytical laboratories performing pH measurements in various fields.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41900886","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 : 2023-04-30DOI: 10.25135/jcm.86.2303.2728
S. H. Ahmadi, H. Daneshyar, N. Dalali
{"title":"Application of the localized surface plasmon resonance of silver nanoparticles for the determination of ethion in water samples","authors":"S. H. Ahmadi, H. Daneshyar, N. Dalali","doi":"10.25135/jcm.86.2303.2728","DOIUrl":"https://doi.org/10.25135/jcm.86.2303.2728","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43902609","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 : 2023-04-28DOI: 10.25135/jcm.85.2303.2727
M. Demirel, Ayşe Zehra Gül, Fatmanur Köktaşoğlu, Halime Ağaç, A. Gören, C. Karatoprak, Ş. Selek
{"title":"1H NMR spectroscopy-based serum metabolomics analysis of iron deficiency anemia","authors":"M. Demirel, Ayşe Zehra Gül, Fatmanur Köktaşoğlu, Halime Ağaç, A. Gören, C. Karatoprak, Ş. Selek","doi":"10.25135/jcm.85.2303.2727","DOIUrl":"https://doi.org/10.25135/jcm.85.2303.2727","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-04-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44057719","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 : 2023-04-04DOI: 10.25135/jcm.83.2301.2676
Alejandro M García Alegría, I. Anduro-Corona, C. J. Pérez-Martínez, Trinidad Quizán-Plata, L. Armenta-Villegas, M. L. Rascón-Durán, H. Astiazarán-García
{"title":"DNA quantification via nanodrop spectrophotometer: estimation of method uncertainty using DNA from standard reference materials, sprague dawley rats, and humans","authors":"Alejandro M García Alegría, I. Anduro-Corona, C. J. Pérez-Martínez, Trinidad Quizán-Plata, L. Armenta-Villegas, M. L. Rascón-Durán, H. Astiazarán-García","doi":"10.25135/jcm.83.2301.2676","DOIUrl":"https://doi.org/10.25135/jcm.83.2301.2676","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46961578","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 : 2023-03-10DOI: 10.25135/jcm.81.2210.2611
P. Khaenamkaew, Chailoek Tanghengjaroen, Dhonluck Manop, Worasit Palkawong Na Ayuthaya, Krirk Wongsontam, Narudom Nualkhow
Analysis of uncertainty estimation for measurement of type and concentration of alcohol in hand sanitisers is a matter of urgency in the COVID-19 situation. FTIR spectroscopy was used to investigate hand sanitisers made in our laboratory and commercial products. An internal standard addition method was used to control the measurement quality. The absorption spectra of ethanol were found to be at 1086 and 1044 cm-1, corresponding to C-O stretching. The area under the C-O adsorptions is used to create a calibration curve, which is then used to calculate the ethanol percentage. Additional standard sample and quality control sample showed calibration curves with slopes of 0.1267 and 0.1285, respectively. The regression coefficients and residual variance of 0.0057 showed a 'best fit' with the predicted value. These parameters were used to estimate the uncertainty of six commercial products. The ethanol concentration of commercial products is measured between 71.38 and 81.54% v/v, with an estimated uncertainty of 1.14% v/v. The results showed that the ethanol content of all products differed from the label but could be used to kill bacteria and viruses. This entire process was established as a SOP for measuring alcohol concentration in hand sanitizer.
{"title":"Assessment of uncertainty estimation for measurement of ethanol concentration in COVID-19 hand sanitizer using FTIR spectroscopy","authors":"P. Khaenamkaew, Chailoek Tanghengjaroen, Dhonluck Manop, Worasit Palkawong Na Ayuthaya, Krirk Wongsontam, Narudom Nualkhow","doi":"10.25135/jcm.81.2210.2611","DOIUrl":"https://doi.org/10.25135/jcm.81.2210.2611","url":null,"abstract":"Analysis of uncertainty estimation for measurement of type and concentration of alcohol in hand sanitisers is a matter of urgency in the COVID-19 situation. FTIR spectroscopy was used to investigate hand sanitisers made in our laboratory and commercial products. An internal standard addition method was used to control the measurement quality. The absorption spectra of ethanol were found to be at 1086 and 1044 cm-1, corresponding to C-O stretching. The area under the C-O adsorptions is used to create a calibration curve, which is then used to calculate the ethanol percentage. Additional standard sample and quality control sample showed calibration curves with slopes of 0.1267 and 0.1285, respectively. The regression coefficients and residual variance of 0.0057 showed a 'best fit' with the predicted value. These parameters were used to estimate the uncertainty of six commercial products. The ethanol concentration of commercial products is measured between 71.38 and 81.54% v/v, with an estimated uncertainty of 1.14% v/v. The results showed that the ethanol content of all products differed from the label but could be used to kill bacteria and viruses. This entire process was established as a SOP for measuring alcohol concentration in hand sanitizer.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43791750","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 : 2023-03-10DOI: 10.25135/jcm.82.2301.2693
R. Kotadiya, Prachi Joshi
: Objectives: The ultraviolet spectrophotometric and reversed-phase high-performance liquid chromatography methods were developed and validated to quantify remogliflozin etabonate and vildagliptin in a fixed-dose tablet formulation. The materials and methods used in this study involved using methanol as the solvent in developing three ultraviolet spectrophotometric techniques, namely simultaneous equation, absorption ratio, and derivative spectroscopy. The wavelength maxima for vildagliptin and remogliflozin etabonate were determined to be 232 nm and 217 nm, respectively. The chromatographic method involved using a Phenomenex Luna C18 column (250 × 4.6 mm, 5 µm) and a mobile phase consisting of a mixture of methanol and acetate buffer (pH 5.6) in a 70:30 ratio. The flow rate was set at 1 mL/min, and the detecting wavelength was 210 nm. The results obtained from the optimized approaches met the performance test criteria set by the International Conference on Harmonization guideline Q2 (R1). The methods were then applied to assay marketed tablet formulations, and the results obtained were within acceptable limits. In conclusion, the developed techniques can be used to analyze the fixed-dose tablet formulation regularly.
：目的：建立并验证了紫外分光光度法和反相高效液相色谱法对固定剂量片剂中的依泊净和维达格利汀进行定量。本研究中使用的材料和方法包括以甲醇为溶剂开发三种紫外分光光度法，即联立方程、吸收比和导数光谱法。维达列汀和瑞格列嗪依他波酸的最大波长分别为232nm和217nm。色谱方法包括使用Phenomenex Luna C18柱（250×4.6 mm，5µm）和流动相，流动相由甲醇和乙酸缓冲液（pH 5.6）的混合物组成，比例为70:30。流速设定为1mL/min，检测波长为210nm。从优化方法中获得的结果符合国际协调会议准则Q2（R1）制定的性能测试标准。然后将这些方法应用于市场上销售的片剂配方的测定，得到的结果在可接受的限度内。总之，所开发的技术可以用于定期分析固定剂量片剂的配方。
{"title":"Simultaneous estimation of remogliflozin etabonate and vildagliptin in a tablet formulation: UV spectrophotometric and HPLC-PDA method","authors":"R. Kotadiya, Prachi Joshi","doi":"10.25135/jcm.82.2301.2693","DOIUrl":"https://doi.org/10.25135/jcm.82.2301.2693","url":null,"abstract":": Objectives: The ultraviolet spectrophotometric and reversed-phase high-performance liquid chromatography methods were developed and validated to quantify remogliflozin etabonate and vildagliptin in a fixed-dose tablet formulation. The materials and methods used in this study involved using methanol as the solvent in developing three ultraviolet spectrophotometric techniques, namely simultaneous equation, absorption ratio, and derivative spectroscopy. The wavelength maxima for vildagliptin and remogliflozin etabonate were determined to be 232 nm and 217 nm, respectively. The chromatographic method involved using a Phenomenex Luna C18 column (250 × 4.6 mm, 5 µm) and a mobile phase consisting of a mixture of methanol and acetate buffer (pH 5.6) in a 70:30 ratio. The flow rate was set at 1 mL/min, and the detecting wavelength was 210 nm. The results obtained from the optimized approaches met the performance test criteria set by the International Conference on Harmonization guideline Q2 (R1). The methods were then applied to assay marketed tablet formulations, and the results obtained were within acceptable limits. In conclusion, the developed techniques can be used to analyze the fixed-dose tablet formulation regularly.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48124890","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 : 2022-12-31DOI: 10.25135/jcm.80.2211.2667
S. Carikci, A. Gören, T. Kilic, T. Dirmenci
AbstrAbstract: Origanum majorana L., (OM), O. onites L. (OO) and O. syriacum L. (subsp. bevanii (Holmes) Greuter & Burdet) (OS) are belong to Majorana (Mill.) Benth. section of Origanum L. genus. In this study, quantities of some phenolic compounds; gallic acid, syringic acid, p -hydory benzoic acid, caffeic acid, ( E )-ferulic acid, chlorogenic acid, rosmarinic acid, pyrogallol and vanillin; in the chloroform (C), acetone (Ac) and methanol (M) extracts prepared from Origanum species collected from Türkiye were investigated via liquid chromatography and tandem mass spectrometry (LC-MS/MS). The relative standard deviations (RSD) of the phenolics were found as follows; 4.85, 8.39, 4.78, 8.04, 5.21, 5.45, 3.73, 5.47, respectively. Curcumin was used as an internal standard. In the extracts, ( E )-ferulic acid and caffeic acid were found to be the most abundant compounds. O. syriacum was determined as the richest species in terms of phenolic acids.
{"title":"Phenolic compounds from section Majorana (Mill.) Benth of Origanum L. species extracts via validated LC-MS/MS method","authors":"S. Carikci, A. Gören, T. Kilic, T. Dirmenci","doi":"10.25135/jcm.80.2211.2667","DOIUrl":"https://doi.org/10.25135/jcm.80.2211.2667","url":null,"abstract":"AbstrAbstract: Origanum majorana L., (OM), O. onites L. (OO) and O. syriacum L. (subsp. bevanii (Holmes) Greuter & Burdet) (OS) are belong to Majorana (Mill.) Benth. section of Origanum L. genus. In this study, quantities of some phenolic compounds; gallic acid, syringic acid, p -hydory benzoic acid, caffeic acid, ( E )-ferulic acid, chlorogenic acid, rosmarinic acid, pyrogallol and vanillin; in the chloroform (C), acetone (Ac) and methanol (M) extracts prepared from Origanum species collected from Türkiye were investigated via liquid chromatography and tandem mass spectrometry (LC-MS/MS). The relative standard deviations (RSD) of the phenolics were found as follows; 4.85, 8.39, 4.78, 8.04, 5.21, 5.45, 3.73, 5.47, respectively. Curcumin was used as an internal standard. In the extracts, ( E )-ferulic acid and caffeic acid were found to be the most abundant compounds. O. syriacum was determined as the richest species in terms of phenolic acids.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43849503","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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