Journal of Chemical Metrology最新文献

{"title":"Validated chromatographic methods for concurrent determination of atorvastatin and perindopril","authors":"Sagar Patel, C. Patel, J. Surati, A. Akabari, K. Shah","doi":"10.25135/jcm.72.2208.2545","DOIUrl":"https://doi.org/10.25135/jcm.72.2208.2545","url":null,"abstract":": Two simple, selective, precise, and accurate chromatographic methods, namely reversed-phase high-performance liquid chromatography (RP-HPLC) method and High-performance thin-layer chromatography (HPTLC), were developed and validated for the simultaneous determination of Atorvastatin (ATO) and Perindopril (PER). The developed HPTLC method was used for the separation and quantitation of the studied drugs on silica gel 60F254 TLC plates. Dichloromethane: Methanol: Ethyl acetate: Glacial acetic acid (6:2:2:0.1, v/v/v/v) was used as a developing system and the separated bands were UV-scanned at 221 nm. Linear relationships were obtained in the range of 800 – 4800 ng/band for Atorvastatin and 200 – 1200 ng/band for Perindopril with a regression coefficient greater than 0.999. The Rf value of the drug was found to be 0.70 ± 0.02 and 0.39 ± 0.03 for Atorvastatin and Perindopril respectively. The developed RP-HPLC depended on chromatographic separation of the studied drugs on a C18 column using Acetonitrile: Methanol: Potassium dihydrogen orthophosphate (pH 3 adjusted with orthophosphoric acid) ((40:10:50), v/v/v) as a mobile phase delivered at a constant flow rate of 1 mL/min with UV detection at 240 nm. The calibration curves were linear (r2 > 0.999) over the concentration range 20-100 µg/mL for Atorvastatin and 10-50µg/mL for Perindopril. The average retention times for Atorvastatin and Perindopril were 3.42 and 8.92 min, respectively. Factors affecting the developed methods have been studied and optimized. Further, methods validation has been carried out according to ICH guidelines. The proposed methods were successfully applied for the determination of the studied drug simultaneously in bulk and synthetic mixture qualitatively and quantitatively. Statistical analysis by the F test showed no significant difference between the results obtained by the two methods. The uncertainty measurement was also carried out for the quantification of both components. The proposed HPTLC method proved to be more sensitive, while the HPLC gave more reproducible results and was time-saving.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-10-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47491515","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 of RP-HPLC PDA method for concurrent quantification of Baloxavir marboxil and its impurities","authors":"Divya Molleti, A. Pawar","doi":"10.25135/jcm.71.2202.2344","DOIUrl":"https://doi.org/10.25135/jcm.71.2202.2344","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43341375","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":"A highly selective and sensitive spectrofluorometric method for quantification of meropenem in its dosage form and fresh human plasma","authors":"A. Fahim, Abbas Alshirify, Kasim Hassan","doi":"10.25135/jcm.70.2202.2363","DOIUrl":"https://doi.org/10.25135/jcm.70.2202.2363","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49437275","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":"Measurement uncertainty assessment for potentiometric determination of trace anionic impurities in graphite post ultrasonic extraction: A bottom-up approach","authors":"H. Parab, Sangita D. Kumar","doi":"10.25135/jcm.69.2202.2367","DOIUrl":"https://doi.org/10.25135/jcm.69.2202.2367","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46997893","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":"Identification, separation and mass spectral characterization of degradants in Cariprazine HCl by LC-MS/MS/QTOF","authors":"Pallekona Sushma, A. Pawar","doi":"10.25135/jcm.68.2201.2338","DOIUrl":"https://doi.org/10.25135/jcm.68.2201.2338","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48551614","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":"LC-HRMS profiling of phytochemicals, antidiabetic, anticholinergic and antioxidant activities of evaporated ethanol extract of Astragalus brachycalyx Fischer","authors":"I. Gülçin, Hatice Kiziltaş, Zeynebe Bi̇ngöl, A. Gören, S. M. Pinar, S. Alwasel","doi":"10.25135/jcm.62.2107.2155","DOIUrl":"https://doi.org/10.25135/jcm.62.2107.2155","url":null,"abstract":"Astragalus is a perennial plant that has existed for about 2500-3000 years and consists of more than 250 taxonomic parts. Twenty species of Astragalus are endemic to Turkey, as well as the richest genus with 425 taxa. The roots of Astragalus species are used in folk medicine as hepatoprotective, antioxidant, antibacterial, antihypertensive, antidiabetic and diuretic. Also, it is used to treat diabetes mellitus, leukemia, nephritis and uterine cancer. It is known that in Anatolia, Astragalus roots are traditionally used against leukemia and wound healing. For the purpose, the measuring of antioxidant activity of evaporated ethanol extract of Astragalus brachycalyx FISCHER (EEAB), some bioanalytic methods including DPPH and ABTS scavenging effects, ferric ions (Fe) and cupric ions (Cu) reducing abilities, and metal (Fe) chelating activity were realized. α-Tocopherol, ascorbic acid, and BHT were used as the standard antioxidants. On the other hand, some phenolic compounds, which responsible for antioxidant activities of EEAB was determined by liquid chromatography-high resolution mass spectrometry (LC-HRMS). At the similar concentration, EEAB exhibited efficient antioxidant effects when compared to standard compounds. Additionally, EEAB showed IC50 values of 1.985 μg/mL toward acetylcholinesterase (AChE), 0.620 μg/mL on α-glycosidase and 0.306 μg/mL against α-amylase enzymes.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":"1 1","pages":""},"PeriodicalIF":1.3,"publicationDate":"2021-12-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41930518","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 of a quality control material for the analysis of volatile compounds in alcoholic beverages","authors":"S. Charapitsa, S. Sytova, A. Kavalenka, L. Sobolenko, Yauheni Shauchenka, N. Kostyuk, M. Zayats, V. Egorov, S. Leschev, I. Melsitova, Siarhei Vetokhin, N. Zayats","doi":"10.25135/jcm.66.2111.2259","DOIUrl":"https://doi.org/10.25135/jcm.66.2111.2259","url":null,"abstract":": A quality control material (QCM) for the analysis of volatile compounds in alcoholic beverages was developed. The problems of the development and production of QCM were investigated. The seven water-ethanol solutions, containing 9 volatile compounds (acetaldehyde, methyl acetate, ethyl acetate, methanol, propan-1-ol, propan-2-ol, 2-methylpropan-1-ol, butan-1-ol and 3-methylbutan-1-ol) with a concentration range from 1.20 to 5000 mg/L of anhydrous ethanol were prepared and studied according to the ISO Guide 80 and ISO Guide 35 in order to prove their stability over 6 months. The algorithm for the assessment of uncertainty associated with the characterization of QCM was developed. The studies were carried out by validated direct gas chromatography (GC) method with flame ionization detection (FID), based on using ethanol as an internal standard. The expanded relative uncertainty of QCM does not exceed 4.5 %.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2021-12-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49547412","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":"SSimultaneous estimation of Pyridoxine HCl and FMOC-Leucine using derivative and chromatographic approach in pharmaceutical dosage form","authors":"Dr Akhil Nagar, Chaitali R Patel, P. Jain, Samadhan J. Shinde, A. Shirkhedkar, Ruchita Bardya","doi":"10.25135/jcm.65.2109.2205","DOIUrl":"https://doi.org/10.25135/jcm.65.2109.2205","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2021-12-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43738207","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":"Characterization of low-density polyethylene reference material for melt flow rate by collaboration of NIS and a network of competent laboratories","authors":"H. Moustafa, Ibrahim F. Tahoun, A. Abou‐Kandil, N. Darwish","doi":"10.25135/jcm.63.2107.2148","DOIUrl":"https://doi.org/10.25135/jcm.63.2107.2148","url":null,"abstract":"The growth rate of plastic manufacturing all over the world and in the middle east as oil producing countries increased the rate of thermoplastics production and the needs of reference materials (RMs) for use in performance evaluation of measuring instruments and ensuring validity of measurement results. This article was focused on the preparation of RM based melt mass-flow rate from low-density polyethylene (LDPE) according to ISO 1133-1 standard. The characterization was evaluated from around 10% of prepared units, then the samples were distributed to a network of collaborating laboratories in order to ensure the validity of the RM production process. The value of melt mass-flow rate of LDPE was determined to be 19.51 g/10 min under a temperature of 190°C and a load of 2.16 kg with expanded uncertainty 0.38 at 95% confidence level. The obtained values were confirmed from the data reported by the network of collaborating laboratories.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2021-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49636082","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":"Quantification of antileukemic drug Dasatinib in human plasma: Application of a sensitive liquid chromatographic method","authors":"Avani Chokshi, A. Gajjar, Pooja Bhanushali, Pritesh Desai","doi":"10.25135/jcm.64.2108-2174","DOIUrl":"https://doi.org/10.25135/jcm.64.2108-2174","url":null,"abstract":"Dasatinib is a tyrosine kinase inhibitor that is approved and prescribed to patients with chronic myelogenous leukemia and Philadelphia chromosome. Present work reports development of reversed-phase high performance liquid chromatographic method for determination of Dasatinib in human plasma and validation of the developed method according to the guidelines provided by European Medicines Agency (EMA). An RP-HPLC method with UV detection and isocratic elution has been developed and validated for analysis of Dasatinib in human plasma over a range of 5-300 ng/mL. Imatinib was used as an internal standard. Both, the drug and the internal standard were separated on the Inertsil C18 column (150 mm×4.6 mm×0.005 mm) using Ammonium Acetate buffer pH 6.4 and acetonitrile at a ratio of 65:35 as mobile phase. The flow rate was adjusted to 0.7 mL min-1. The detection was performed at 310 nm wavelength. Sample pre-purification was performed through simple protein precipitation using acetonitrile followed by sample collection through centrifugation. The developed method was linear in the range of 5-300 ng/mL with correlation coefficients (r) of 0.995. The lower limit of quantification for Dasatinib in plasma was 5 ng/mL. The accuracy and precision of the method were well within the acceptable limits of 15% over the linear range. In general, the developed method is efficient and inexpensive. It is very simple from the extraction of drug from the plasma matrix to the isocratic elution of analytes. From the data, it can be concluded that the developed method is selective, precise and accurate and applicable for the determination of Dasatinib in human plasma samples.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2021-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44559169","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}