Journal of Chemical Metrology
A scientific open access journal in the field of analytical chemistry and accreditation
Journal of Chemical MetrologyA scientific open access journal in the field of analytical chemistry and accreditation
Certification of sodium benzoate solution reference material by HPLC-UV, LC-MS/MS and UV-VIS-NIR spectrophotometry for food and drug analysis
Sodium benzoate is one of the most widely used food perseverates and has to be used in regulated amounts to avoid its harmful health effects. Reviewing the scientific literature for traceability of the analytical measurement results of sodium benzoate in various food and drug applications to the SI units, it has been found that no scientific details of certification of sodium benzoate CRMs used for the calibration of measuring equipment are published. For this reason, the national metrology institute of Saudi Arabia (SASO/NMCC) certifies a sodium benzoate solution reference material. In this work, sodium benzoate was synthesized, purified and a batch solution reference material was prepared as 1014.47 mg/kg then homogenized and bottled. Homogeneity and stability of the candidate RM were assessed and the results obtained showed that the material is sufficiently homogeneous and stable. Characterization of the reference material was carried out by HPLC-UV, LC-MS/MS and UV-VIS-NIR spectrophotometer as three independent methods. The certified value was derived by combining data from the three methods using the weighted mean approach and was found 1016.13 mg/kg. The certified uncertainty was calculated as weighted uncertainty and was found 10.47 mg/kg (1.03%). Sources of this uncertainty were identified from the characterization, uchar, homogeneity, uhom, and long-term stability, ults, as well as the bias allowance, B.DOI http://doi.org/10.25135/jcm.48.20.08.1780 (DOI number will be activated after the manuscript has been available in an issue.) Keywords CRM sodium benzoate homogeneity stability characterization certified value Available online: October 18, 2020 DETAILS DOWNLOAD PDF © ACG Publications. All rights reserved.
UV-spectrophotometry-assisted chemometric methods for simultaneous determination of ambroxol hydrochloride and doxofylline in pharmaceutical formulation
Two methods, ratio spectra derivative method and partial least squares regression (PLS) were developed for the simultaneous estimation of ambroxol hydrochloride and doxofylline in combined dosage form. In the first method, ratio spectra derivative method, analytical signals were measured at the wavelengths corresponding to either maximums or minimums for both drugs in the first derivative spectra of the ratio spectra obtained by dividing the standard spectrum of one of two drugs in water. Partial least squares regression (PLS) was used for data analysis of and the parameters of the chemometry procedures were optimized. In this study, the simultaneous determination of ambroxol hydrochloride and doxofylline in pharmaceuticals by chemometric approaches using UV spectrophotometry has been reported. Spectra of ABH and DOX were recorded at several concentrations within their linear ranges between 2-12 μg/mL and 15-40 μg/mL respectively and applied to pharmaceutical formulation, tablet, with no interference with excipients as indicated by the results of the recovery study. The proposed methods are simple, rapid and can be easily used in the quality control of drugs as alternative analytical tools.DOI http://doi.org/10.25135/jcm.47.20.05.1638 (DOI number will be activated after the manuscript has been available in an issue.) Keywords Ambroxol hydrochloride doxofylline partial least squares ratio derivative spectrophotometry Validation Available online: October 05, 2020 DETAILS DOWNLOAD PDF © ACG Publications. All rights reserved.
Stability indicating liquid chromatographic method for the estimation of remogliflozin etabonate
Accurate and precise reverse phase liquid chromatographic method has been developed for the estimation Remogliflozin etabonate in bulk and tablet dosage form. Reverse phase C18 column was used as stationary phase along with mixture of methanol:water (70:30%, v/v) as a mobile phase. Mobile phase flow rate was maintained at 1mL/min and analysis was performed at 229 nm. The method was linear in the concentration range of 1 – 25 μg/mL with correlation coefficient (r2) 0.997. The proposed method was validated with respect to linearity, accuracy, precision and robustness as per ICH Q2 (R1) guideline. To find out the possible degradation pathway, forced degradation studies were performed. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time value. The drug was found to be highly susceptible to acid and base hydrolysis. The developed method can be used for analysis of stability samples and routing quality control evaluation of Remogliflozin etabonate in tablet formulation.DOI http://doi.org/10.25135/jcm.46.20.07.1734 (DOI number will be activated after the manuscript has been available in an issue.) Keywords Forced Degradation validation remogliflozin liquid chromatography Available online: October 02, 2020 DETAILS DOWNLOAD PDF © ACG Publications. All rights reserved.
Development of TLC method for simultaneous estimation of novel combination of amlodipine besylate, rosuvastatin calcium, and fimasartan potassium in synthetic mixture
An accurate, sensitive, robust and precise high performance thin layer liquid chromatography method was developed based on ICH Q2 (R1) guidelines for estimation of novel combination of Amlodipine besylate, Rosuvastatin calcium and Fimasartan potassium in bulk and its synthetic mixture. Pre-coated silica gel aluminum plate 60 F254 was selected as the stationary phase and n-hexane, n-butanol, methanol, and Glacial Acetic Acid (5.7:2:2.3:0.1, v/v/v/v) was selected as mobile phase. All three drugs showing appreciable absorbance at the common wavelength of 242 nm were selected for quantification of Amlodipine besylate, Rosuvastatin calcium, and Fimasartan potassium, respectively. The method was validated for linearity, precision, accuracy, and robustness, limit of detection and limit of quantitation as per ICH parameters. The regression coefficients (r2) were found to be 0.9986, 0.9975 and 0.9988 for Amlodipine besylate, Rosuvastatin calcium, and Fimasartan potassium, respectively. The average percentage recovery of Amlodipine besylate, Rosuvastatin calcium and Fimasartan potassium were found to be 99.38-100-60%, 99.75-100.63%, 99.39-100%, respectively. Thin Layer Chromatographic method has prospective qualitative as well as quantitative applications for concurrent estimation of Amlodipine besylate, Rosuvastatin calcium and Fimasartan potassium in bulk and pharmaceutical dosage form.DOI http://doi.org/10.25135/jcm.45.20.07.1744 (DOI number will be activated after the manuscript has been available in an issue.) Keywords HPTLC; amlodipine besylate (AML); rosuvastatin calcium(ROS); fimasartan potassium (FIM); validation Available online: September 28, 2020 DETAILS DOWNLOAD PDF © ACG Publications. All rights reserved.