A Simple and Cost-Effective TLC-Densitometric Method for the Quantitative Determination of Acetylsalicylic Acid and Ascorbic Acid in Combined Effervescent Tablets
Abstract:A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validat… Show more
“…Limit of detection and quantification was determined by preparing three standard solutions of valproic acid at concentration of 15, 10, and 7.5 mg/5 mL (in the case of valproic acid detected with 2% CuSO 4 solution), and three standard solutions of valproic acid at concentration of 1.0, 0.9, and 0.8 mg/5 mL (in the case of valproic acid detected by the 2 ,7 -dichlorofluorescein-aluminum chloride-iron [III] chloride system). The LOD and LOQ calculation methodology was given in our earlier works [47][48][49]. The analyses were repeated three times.…”
Section: Limit Of Detection (Lod) and Limit Of Quantification (Loq)mentioning
Determination of valproic acid in the drug was carried out on the aluminum silica gel 60F254 plates and using acetone–water–chloroform–ethanol–ammonia at a volume ratio of 30:1:8:5:11 as the mobile phase, respectively. Two methods of detection of valproic acid were used. The first was a 2% aqueous CuSO4×5H2O solution, and the second was a 2′,7′-dichlorofluorescein-aluminum chloride-iron (III) chloride system. The applied TLC-densitometric method is selective, linear, accurate, precise, and robust, regardless of the visualizing reagent used for the determination of valproic acid in Convulex capsules. It has low limits of detection (LOD) and limits of quantification (LOQ), which are equal to 5.8 μg/spot and 17.4 μg/spot using a 2% aqueous CuSO4×5H2O solution as visualizing agent and also 0.32 μg/spot and 0.97 μg/spot using a 2′,7′-dichlorofluorescein-aluminum chloride-iron (III) chloride system as visualizing reagent, respectively. The described analytical method can additionally be used to study the identity of valproic acid in a pharmaceutical preparation. The linearity range was found to be 20.00–80.00 μg/spot and 1.00–2.00 μg/spot for valproic acid detected on chromatographic plates using a 2% aqueous CuSO4×5H2O solution and the 2′,7′-dichlorofluorescein-aluminum chloride-iron (III) chloride system, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of valproic acid equal 96.2% and 97.0% in relation to the label claim that valproic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine analysis of valproic acid in pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography and square wave voltammetry in the control of above-mentioned substances, and it can be applied when other analytical techniques is not affordable in the laboratory.
“…Limit of detection and quantification was determined by preparing three standard solutions of valproic acid at concentration of 15, 10, and 7.5 mg/5 mL (in the case of valproic acid detected with 2% CuSO 4 solution), and three standard solutions of valproic acid at concentration of 1.0, 0.9, and 0.8 mg/5 mL (in the case of valproic acid detected by the 2 ,7 -dichlorofluorescein-aluminum chloride-iron [III] chloride system). The LOD and LOQ calculation methodology was given in our earlier works [47][48][49]. The analyses were repeated three times.…”
Section: Limit Of Detection (Lod) and Limit Of Quantification (Loq)mentioning
Determination of valproic acid in the drug was carried out on the aluminum silica gel 60F254 plates and using acetone–water–chloroform–ethanol–ammonia at a volume ratio of 30:1:8:5:11 as the mobile phase, respectively. Two methods of detection of valproic acid were used. The first was a 2% aqueous CuSO4×5H2O solution, and the second was a 2′,7′-dichlorofluorescein-aluminum chloride-iron (III) chloride system. The applied TLC-densitometric method is selective, linear, accurate, precise, and robust, regardless of the visualizing reagent used for the determination of valproic acid in Convulex capsules. It has low limits of detection (LOD) and limits of quantification (LOQ), which are equal to 5.8 μg/spot and 17.4 μg/spot using a 2% aqueous CuSO4×5H2O solution as visualizing agent and also 0.32 μg/spot and 0.97 μg/spot using a 2′,7′-dichlorofluorescein-aluminum chloride-iron (III) chloride system as visualizing reagent, respectively. The described analytical method can additionally be used to study the identity of valproic acid in a pharmaceutical preparation. The linearity range was found to be 20.00–80.00 μg/spot and 1.00–2.00 μg/spot for valproic acid detected on chromatographic plates using a 2% aqueous CuSO4×5H2O solution and the 2′,7′-dichlorofluorescein-aluminum chloride-iron (III) chloride system, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of valproic acid equal 96.2% and 97.0% in relation to the label claim that valproic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine analysis of valproic acid in pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography and square wave voltammetry in the control of above-mentioned substances, and it can be applied when other analytical techniques is not affordable in the laboratory.
The potentiometric titration (PT) method has been applied for the first time to investigate the stability of L-ascorbic acid (H2Asc) and to determine its degradation products in aqueous solutions. The presented electrochemical procedures can be considered to be a fast, simple and inexpensive way to control the stability of H2Asc in a regular analytical practice as well as in the chemical and pharmaceutical industries. Experimental data as well as modeling suggest that the enolic form of 2,3-diketogulonic acid predominates in a solution as the main product of dehydroascorbate (DHA) degradation. Furthermore, the PT results supported by conductometric measurements (CM) and electrospray ionization mass spectrometry (ESI/MS) data enable us to propose the putative mechanism of the H2Asc decomposition. Moreover, it has been proven that among different types of investigated electrolytes (KNO3, KClO4 and KSCN), the thiocyanate ions (SCN-) reveal the stabilizing effect against the degradation of H2Asc. Thus, the presence of SCN- in the H2Asc solution is proposed as an alternative way for some organic solvents earlier used. Finally, a new paraffin-protection-layer procedure has been recommended for studying as well as storage of the solutions comprising components sensitive to external factors (e.g. O2, CO2) and to evaporation.
“…There is a lot of toxicants added in milk as adulteration by using nanotechnology the recent research is emphasizing on, salicylic acid (C 7 H 6 O) which is known to be added in milk as a preservative in order to enhance shelf life and is associated with gastric irritation, bleeding, diarrhea, renal disease and even death in mammals (Nagraik et al, 2021). Traditional detection methods of salicylic acid (SA) include high-end advanced instruments that are LCMS (Liquid Chromatography-Mass Spectrometry) (Protasiuk & Olejnik, 2018), Gas Chromatography-Mass Spectroscopy (Božić Luburić et al, 2022) TLC, and High-Performance Liquid Chromatography (Pyka-Pająk et al, 2018).…”
The highly selective, sensitive, and quick interference green synthesis-based sensing of possible milk adulterants i.e., salicylic acid has been reported here. Salicylic acid interacts with nanoparticles through strong bonding interactions, hence resulting in an interruption within the formation of selenium nanoparticles which is confirmed by UV-VIS spectroscopy, scanning electron microscopy, and x-ray diffraction. This interaction in the synthesis of nanoparticles resulted in transmittance wavelength that decrease with the increasing amount of salicylic acid, showing strong binding of selenium nanoparticles with adulterant thereby permitting in-situ fast detection of salicylic acid from milk having a limit of detection at 10 -3 mol and linear coefficient correlation of 0.9907.
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