scholarly journals Separation of Sb (V) and Sb (III) antimony compounds using anion exchange chromatography technique

2020 ◽  
Vol 12 (3) ◽  
pp. 164-169
Author(s):  
Herlinawati Herlinawati ◽  
◽  
Buchari Buchari ◽  
M. Bachri Amran ◽  
◽  
...  

Separation of Sb (V) and Sb (III) antimony compounds using anion exchange chromatography technique have been done. To obtain the separation of Sb (V) and Sb (III) antimony compounds which is good in this study have been studied several parameters of separation in anion exchange chromatography technique. Parameters that influence the process of separation of Sb (V) and Sb (III) antimony compounds is the concentration and pH of the mobile phase (eluent) have been evaluated. The separation of Sb (V) and Sb (III) antimony compounds is good and optimum obtained using an eluent 200 mM phosphate buffer at pH 7 with a flow rate of 1 mL/min. Based on the optimum conditions for the separation of Sb (V) and Sb (III) antimony compounds with anion exchange chromatography method has generated value the capacity factor (k ') Sb (V) and Sb (III) obtained are respectively 1.77 and 3.01. While the value of selectivity (α), Number of theoretical plates (N) and Resolution (Rs) obtained are respectively 1.70; 369.48; and 1.48.

2018 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Dwi Karina Natalia ◽  
Harmita . ◽  
Taufiq Indra Rukmana

Objective: This study aimed to develop a selective analytical method for assessing disodium 5′-guanylate and disodium 5′-inosinate levels in flavorenhancers.Methods: The levels were assessed using high-performance liquid chromatography (HPLC) with a photodiode array detector (PDA) (wavelength=255 nm) and a SunFire® C18 column (250 mm × 4.6 mm × 5 μm). The mobile phase comprised a mixture of potassium phosphate buffer and anion pair reagent-hexane-1-sulfonic acid sodium salt - with a flow rate of 1.2 mL/min. The ion pair was used to generate a neutral equilibrium, whichresulted in increased retention of the analytes. Optimized analysis conditions were then validated regarding accuracy, precision, linearity, selectivity,and the limits of detection and quantification.Results: The average levels of disodium 5′-inosinate in the six analyzed samples were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and0.47±2.21%, respectively. Regarding disodium 5′-guanylate, the average levels were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and0.34±1.83, respectively.Conclusion: The optimal conditions for analyzing disodium 5′-guanylate and disodium 5′-inosinateusing HPLC with a PDA and SunFire C18 columnwere λ=255 nm, a mobile phase of potassium phosphate buffer and sodium hexane sulfonate, and a flow rate of 1.2 mL/min. For disodium 5′-inosinate,its average levels in samples A–F were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and 0.47±2.21%, respectively. Meanwhile, the averagelevels of disodium 5′-guanylate in the samples were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and 0.34±1.83%, respectively.


2019 ◽  
Vol 102 (5) ◽  
pp. 1523-1529
Author(s):  
Şule Dinç-Zor ◽  
Bürge Aşçi ◽  
Özlem Aksu Dönmez ◽  
Özge Hacimustafa

Abstract Background: Preservatives and colorants in pharmaceutical products may be highly toxic, especially for sensitive individuals, when they are used in excessive amounts. In this context, sensitive and non-labor-intensive analytical methods with short analysis time for simultaneous quantification of these additive substances in drugs can meet all requirements in quality control laboratories. Objective: The aim of the study was to develop a simultaneous HPLC method for the analysis of pseudoephedrine HCl and guaifenesin, along with preservatives, methyl paraben and propyl paraben, and colorants, ponceau 4R and sunset yellow, in a syrup sample. Methods: Optimum conditions of HPLC separation were determined by Box-Behnken experimental design. Four independent variables of the separation were pH (6.0, 6.5, and 7.0) and flow rate of the mobile phase (2.0, 2.2, and 2.4 mL/min) and mobile phase ratios for the first and second gradient elutions (75, 80, and 85% for Gradient 1 and 50, 55, and 60% for Gradient 2 in terms of phosphate buffer percent, respectively). Results: The optimum conditions were found to be pH, 6.3; flow rate, 2.4 mL/min; and mobile phase ratios (phosphate buffer-acetonitrile) for Gradient 1 and 2, 85+15 (v/v) and 60+40 (v/v), respectively. Conclusions: Simultaneous analysis of all compounds was achieved by using this HPLC method with a short run time below 10 min. Highlights: This simple, rapid, and validated method is convenient and applicable for routine analysis of pharmaceutical products having similar composition without the need for any extraction step.


2018 ◽  
Vol 2018 ◽  
pp. 1-6 ◽  
Author(s):  
Lidong Cao ◽  
Huifang Tian ◽  
Miaomiao Wu ◽  
Hongjun Zhang ◽  
Puguo Zhou ◽  
...  

The increasing interest of curdlan oligosaccharides (COS) in medicine and plant protection fields implies a necessity to identify and quantify this product. In the present study, an efficient and sensitive analytical method based on high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) was established for the simultaneous separation and determination of D-glucose and ß-1,3-linked COS ranging from (COS)2 to (COS)6 within 20 min. Detection limits were 0.01 to 0.03 mg/L. The optimized assay was performed on a CarboPac-PA100 analytical column (4 mm × 250 mm) using isocratic elution with water−0.2 M sodium hydroxide−0.5 M sodium acetate mixture (50 : 30 : 20, v/v/v) as the mobile phase at a flow rate of 0.8 mL/min. Regression equations indicated a good linear relationship (R2 = 0.9992–1.0000, n = 6) within the test ranges. Quality parameters including precision and accuracy were fully validated and found to be satisfactory. More important, the regression of natural logarithm values of retention times (log10 RT) versus the degree polymerization (DP), as well as the slope coefficient of each COS’s linear equation versus the corresponding DP, fitted a linear relationship well. These inherent linear relationships could provide valuable information to tentatively identify and quantify the COS even with the DP more than 6 without authentic standard. Furthermore, when the log10 RT was plotted against log10 flow rate for each COS, a perfect linear relationship was also observed.


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