Determination Of Trometamol Content In Gadobutrol Solution For Intravenous Administration, 1 mmol / mL Using RP-LC With Refractive Index Detector

Background: Extremely responsive technique designed for the willpower of trometamol for instance tris(hydroxymethyl)aminomethane in gadobutrol by RP-LC technique. Quantification of trometamol content in gadobutrol samples by HPLC with refractive index detector (RID). Trometamol was UV inactive compound.Methods: Trometamol was determined by RP-LC method using Inertsil NH2 (250x4.6mm, 5µm) column as motionless segment. Column temperature maintained 30°C, inoculation quantity 10µL, flow velocity was 0.3 ml/min, sample cooler temperature 25°C. The mixture of phosphate buffer and cyanomethane in the ratio of 990:10 (volume/volume) was utilized as movable segment. The retention time of trometamol determined 10.95 minutes respectively. The acceptance limit of the trometamol content is 0.9%-1.5%.ConclusionThe proposed RP-LC technique that can determination of trometamol content in gadobutrol solution intravenous administration contain expanded as well as authenticated as per ICH guidelines. The efficiency of the technique was ensure by the specificity, exactitude and accuracy. Hence, the technique well suit for their intended purposes and can be productively useful for the release testing of gadobutrol injection keen on the souk.

Direct determination of cellulosic glucan content in starch-containing samples

A simple and highly selective analytical procedure is presented for the determination of cellulosic glucan content in samples that contain both cellulose and starch. This method eliminates the unacceptably large compounding errors of current two-measurement methods. If both starch and cellulose are present before analytical hydrolysis, both will be hydrolyzed to glucose causing bias and inaccuracy in the method. To prevent this interference, the removal of starch prior to cellulosic quantification is crucial. The method presented here is a concise in-series procedure with minimal measurements, eliminating large compounding errors. Sample preparation consists of a starch extraction employing enzymatic hydrolysis followed by a simple filtration and wash. The samples are then subjected to a two-stage acid hydrolysis. The concentration of glucose is determined by ion exchange high-performance liquid chromatography with a Pb2+ column and a refractive index detector. The cellulosic glucan content is calculated based on the initial dry weight of the starting material. Data for the native biomass materials studied show excellent reproducibility, with coefficients of variance of 3.0% or less associated with the method. This selectivity for cellulosic glucan by the procedure was validated with several analytical techniques such as liquid chromatography coupled with mass spectrometry (LC–MS), Raman spectroscopy, and nuclear magnetic resonance.

The Production of Bioethanol from Carob Pods (Ceratonia siliqua L.)

This study seeks to investigate the use of carob (Ceratonia siliqua. L) as a potential source of bioethanol production. In addition, an attempt to optimize the method through sulfuric acid hydrolysis was carried out and the optimum pH range for carob fermentation was studied at pH 2.5, 4.5 and 7.5. Samples of both foreign and locally originating carob were used and any discrepancy in fermentation performance with respect to origin was noted. Each fermentation setup was prepared with 66 gL-1 carob powder, inoculated with 1gL-1 Saccharomyces cerevisiae yeast strain and supplemented with 0.6 mgL-1 thiamine hydrochloride. A total of 36 fermentation broth samples taken at 24-hour time intervals were analysed for different fermentation variables to monitor the progression of fermentation. Changes in total acidity and reducing sugar were analysed through titration techniques and pH. A quantitative sugar profile based on fructose, glucose and sucrose was constructed using an in-house validated method by HPLC-Refractive Index detector. Ethanolic content of the fermentation broth was determined through an in-house validated method by HPLC-UV detector. A significant change (p < 0.05) in ethanol content across time, was detected, with the highest ethanol concentration being achieved in the unhydrolysed control sample with 1.19% v/v from 66gL-1 carob powder.

Full optimization and validation of an HPLC method for the quantitative analysis of total sugars in a soft drink

Five HPLC methods were employed for the quantitative analysis of three natural sugars namely fructose, glucose and sucrose in soft drinks. HPLC-refractive index detector (RID)-AMINO proved to be the most suitable HPLC method to carry out the latter task. For the optimum separation and response of the natural sugars the best conditions employed were column oven temperature 30 oC, flow rate 0.1 mL/min, mobile phase ratio acetonitrile:water 75:25 and they were determined by studying all possible interactions among these three parameters. Full validation of HPLC-RID-AMINO was performed in terms of system suitability test, precision check, accuracy check and robustness. KEY WORDS: Sugar, Soft drink, Experimental design, Validation, HPLC, System suitability Bull. Chem. Soc. Ethiop. 2020, 34(2), 419-426 DOI: https://dx.doi.org/10.4314/bcse.v34i2.17

High-Performance Liquid Chromatography Determination of Free Sugars and Mannitol in Mushrooms Using Corona Charged Aerosol Detection

Refractive index detector is usually used in the analysis of sugars in mushrooms, which is characterized by poor sensitivity, reproducibility, and susceptibility to interference from co-eluting sample components. In the current study, identification and determination of free sugars in mushroom samples by high-performance liquid chromatography coupled to corona charged aerosol detector (HPLC-CAD) were presented for the first time. The best chromatographic separation was performed on a Shodex Asahipak NH2P-50 4E 5 μm and mobile phase composed of 75% acetonitrile and 25% water with flow rate was 1 mL/min. The developed method offers good linearity in concentration range 0.001–0.01 or 0.01–0.2 mg/mL for tested compounds with R2 > 0.99. Limit of detection (LOD) for analytes was in the range of 7.1–120.2 ng on column. HPLC-CAD method showed very good reproducibility (RSD < 5.1%). Fructose, mannitol, and glucose were detected in all examined mushroom samples. For white Agaricus bisporus, mannitol was the most abundant sugar (7.575 mg/g dw), whereas trehalose for Pleurotus ostreatus (3.426 mg/g dw). The developed method was successfully applied for quantification of free sugars and mannitol in mushrooms. The optimized method proved to be sensitive, reproducible, and accurate.

Novel Eco-friendly HPLC Methods Using Refractive Index Detector for Analysis of Three Veterinary Antibiotics in Pharmaceutical Formulations and Rat Plasma

Antibiotic resistance increases the human mortality rate nowadays. The main purpose of the present study was to develop green reversed-phase high-performance liquid chromatography (RP-HPLC) methods with a refractive index detector for the assay of the three veterinary antibiotics (VAs), i.e., maduramicin ammonium (MA), apramycin sulfate (AS) and clarithromycin (CLA) in pharmaceutical dosage forms and spiked rat plasma. The method utilized isocratic elution using an ODP-40 C18 column, the flow rate was set at 1.0 mL/min and negative polar signals. The linearity ranges were 3.0–18.0 μg/mL for MA, 1.5–4.0 μg/mL for AS and 0.5 to 3.0 μg/mL for CLA, respectively. Liquid-liquid extraction (LLE) procedure was optimized in plasma samples. The recoveries percentages were 85.4, 81.2 and 88.8 correspondingly, in rat plasma. However, the drugs extraction by protein precipitation method yields very poor recoveries (around 50%). The new HPLC- refractive index (RI) methods are better than the previously reported HPLC-ultra violet methods in terms of greenness and simplicity of procedures. Moreover, the previously reported LC–MS methods lack the simplicity and availability of such expensive techniques in Quality control (QC) labs. The novelty of this research is the use of refractive index detector for the first time for VAs analysis.

Development and Validation of a Novel Reversed Phase High Performance Liquid Chromatography with Refractive Index Detector Method for Assay of Polyvinyl Alcohol in an Ophthalmic Solution

Introduction: Polyvinyl alcohol (PVA), a polymer, is in demand due to its usage in different applications such as pharmaceutical, biomedical and textile, paper, food industries. Methods: A new sensitive reversed phased high-pressure liquid chromatography (RP-HPLC) method with refractive index detector (RID) was developed for determination of PVA in an ophthalmic solution containing dexpanthenol and PVA as active substances and it was validated according to The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guideline. Results: Chromatographic separation was achieved on a Chiral-AGP (150 mm × 4.0 mm, 5 μm) column kept at 30°C with an isocratic flow at a flow rate of 1.0 ml/min. The detector temperature was 30°C, the retention time of PVA was around 1.0 min and the total run time was 5 minutes. Conclusion: The proposed method showed linearity, accuracy, precision, specificity, robustness, solution stability, and system suitability results within the acceptance criteria.