Separation Of Salicylic Acid Research Articles

Selective adsorption and separation of salicylic acid and 4‐hydroxyisophthalic acid from industry‐grade 4‐hydroxybenzoic acid on UiO‐66

AbstractIn this study, UiO‐66 was employed for the first time as an adsorbent to separate phenolic acid analogues, specifically 4‐hydroxyisophthalic acid and salicylic acid, from impurities. Synthesized in‐house, UiO‐66 was shown to exhibit high selectivity towards 4‐HIPA/4‐HBA and SA/4‐HBA when a molar equivalent of acetic acid modulator to terephthalic acid was set at 44. The adsorption capacities for 4‐HBA, 4‐HIPA, and SA were determined to be 56.34, 55.02, and 60.34 mg/g, respectively. Furthermore, it was observed that after six regeneration cycles, the adsorption capacity for 4‐HBA remained nearly unchanged, whereas those for 4‐HIPA and SA decreased by 5.6% and 2.6%, respectively. FTIR and XPS analyses revealed that all three compounds were adsorbed at the same dominant Zr cluster site on UiO‐66, primarily through hydrogen bonding and electrostatic interaction. Dynamic adsorption experiments revealed that 4‐HBA was the first to elute, maintaining the residual contents of 4‐HIPA and SA below 0.1 wt%. Compared to traditional separation techniques, this paper provided a simple and effective method to purify industrial grade 4‐hydroxybenzoic acid.

Separation of salicylic acid and two phenols by polyvinyl chloride/N,N-bis (1-methylheptyl) acetamide polymer inclusion membrane

The separation behaviour and mass transfer mechanism of salicylic acid (SA) and two phenols by a polymer inclusion membrane (PN-PIM) based on polyvinyl chloride (PVC) as a base polymer and N,N-bis (1-methylheptanyl) acetamide (N503) as a carrier were studied. The correlation between the effects of carrier content and membrane thickness on the morphology, structure and mass transfer stability of PN-PIM was discussed. PN-PIM presented a good mass transfer capability for SA and p-nitrophenol (PNP) through a hydrogen transfer mechanism in weakly acidic environments and with low-concentration NaOH as a stripping phase. The mass transfer rate was in accordance with the first-order kinetic equation. At pH 6, the phenol and PNP coexisting with SA can be selectively removed. The mass transfer of PNP in PN-PIM was consistent with the diffusion mechanism, whereas that of SA exhibited the characteristics of a fixed-site hopping mechanism. When the carrier content was 68.8 %, the permeability coefficient (P) of PNP and SA reached at 9.02 and 8.74 μm/s, respectively. The mass transfer activation energies of PNP and SA totalled 13.23 and 19.08 kJ/mol, respectively. Moreover, intramembrane diffusion was the main controlling step of the mass transfer of PNP and SA in PN-PIM. Given the dual effects of PN-PIM membrane thickness on mass transfer stability and mass transfer rate, the suitable thickness range of PN-PIM was 160–180 μm.

Development of new procedures for the detection and separation of salicylic acid and acetylsalicylic acid using thin-layer chromatography with densitometry

Salicylic acid and its derivatives, such as acetylsalicylic acid, are commonly used non-steroidal anti-inflammatory agents. In the present work, different sorbents as the stationary phases and also various manners of detection using well known and new visualizing reagents have been tested for the separation and detection of the two compounds by adsorption and also partition thin-layer chromatography (TLC) with densitometry. Densitometric and spectrodensitometric analysis was used to evaluate the detectability of the examined compounds using the newly developed TLC procedures. Of all the applied manners of detection, the most universal to distinguish acetylsalicylic acid from salicylic acid in normal- as well as in reversed-phase TLC system is the use of methanolic solution of FeCl3 and CoCl2. The densitograms obtained under these conditions show symmetric and also by adsorption well separated TLC peaks of both compounds. The shape of all absorption bands of acetylsalicylic acid (ASA) and 2-hydroxybenzoic ...

Determination of salicylic acid using a magnetic iron oxide nanoparticle-based solid-phase extraction procedure followed by an online concentration technique through micellar electrokinetic capillary chromatography

In this study, a magnetic iron oxide nanoparticle-based solid-phase extraction procedure combined with the online concentration and separation of salicylic acid (SA) through micellar electrokinetic chromatography–UV detection (MEKC–UV) was developed. Under optimal experimental conditions, a good linearity in the range of 0.01–100μmolL−1 was obtained with a coefficient of correlation of 0.9999. The detection sensitivity of the proposed method exhibited an approximately 1026-fold improvement compared with a single MEKC method without online concentration, and the detection limit (S/N=3) was 3.80nmolL−1. The repeatability of the method was evaluated using intraday and interday RSDs (11.5% and 17.0%, respectively). The method was used to determine SA concentrations in tobacco leaves (Nicotiana tabacum L. cv. Samsun) from the NN genotype, nn genotype, and Nt-NahG mutant strains, as well as in shampoo and ointment samples. Rapid extraction and separation (<50min), acceptable repeatability (RSD<17.0%), and high spiked recoveries (95.8%–102.4%) were observed for plants, detergents, and pharmaceuticals.

The use of similarity analysis for evaluation of the chromatographic separation of salicylic acid and its selected derivatives studied by adsorption and partition thin-layer chromatography techniques

The aim of the work was the chromatographic separation of salicylic acid and their derivatives, i.e., acetylsalicylic acid, salicylanilide, salicylaldehyde, salicylamide, methyl salicylate, phenyl salicylate, 2,5-dihydroxybenzoic acid, salicylhydroxamic acid, 3,5-dinitrosalicylic acid, 3-aminosalicylic acid, 4-aminosalicylic acid, and 5-aminosalicylic acid by use of adsorption thin-layer chromatography (normal-phase thin-layer chromatography [NPTLC]) and partition thin-layer chromatography (reversed-phase thin-layer chromatography/high-performance thin-layer chromatography [RP-TLC/HPTLC]). Three qualitatively and quantitatively different mobile phases were used for the separation of salicylic acid and its derivatives. Cluster analysis (single linkage method, Euclidean distance) allowed the evaluation of the suitability of the chromatographic conditions used to separate the pairs of tested compounds. The cluster analysis data indicate that the composition of the mobile phase is fundamental in the process o...

High-performance thin-layer chromatographic analysis of salicylic acid in release medium during development of an adhesive topical anti-acne patch

High-performance liquid chromatography (HPLC) has been the most popular choice for the determination of salicylic acid. This paper describes a method of normal phase isocratic planar chromatography on silica gel 60 F254 high-performance thin-layer chromatography (HPTLC) layer and measurement of fluorescence quenched zones by ultraviolet absorption scanning densitometry at 270 nm for separation of salicylic acid from dissolution media constituents. The established procedure was validated in terms of limit of detection (LOD), limit of quantitation (LOQ), linearity, recovery, and precision. The calibration function of the analyte was linear in the range 57–399 ng zone−1, and the correlation coefficient was 0.999. The limits of detection and quantitation were 25 and 57 ng zone−1. The relative standard deviations were less than 4.0% for repeatability and intermediate precision studies. The recovery was 96.8–103%.

Micellar electrokinetic capillary chromatographic determination of a polypill combination containing, lisinopril, hydrochlorothiazide, aspirin, and atorvastatin

A simple, precise, and rapid micellar electrokinetic capillary chromatographic method with a photodiode array detector was developed and validated for the separation and simultaneous determination of a cardiovascular innovative polypill combination. The combined polypill components were: lisinopril (LIS), hydrochlorothiazide (HCT), aspirin (ASP), and atorvastatin (ATO). Separation was achieved utilizing a fused silica capillary (58 cm × 75 μm ID) and a background electrolyte solution consisting of borax buffer (20 mM, pH 9.5) containing 30 mM sodium lauryl sulphate, with paracetamol as the internal standard. The method was fully validated as per the guidelines of the International Conference on Harmonization for validation of analytical procedures. The method was linear over the range 0.1–200 μg mL−1 with detection limits of 3.10, 0.33, 0.74, and 0.84 μg mL−1 for LIS, HCT, ASP, and ATO, respectively. The proposed method was successfully applied for the simultaneous determination of the polypill components without interferences from the common pharmaceutical excipients. The percentage recoveries of the four drugs from the polypill were 100.07 ± 0.81, 100.30 ± 0.21, 99.73 ± 0.40, and 99.23 ± 0.49% for LIS, HCT, ASP, and ATO, respectively. The method is rapid as it involved a short run time; all the components were eluted within 8 min. Moreover, the method also permitted the separation of salicylic acid which is commonly present in aged aspirin formulations. The results demonstrated that the proposed method has a great practical value for routine application in quality control laboratories for the high-throughput simultaneous determination of the polypill components.

Electro-Membrane Process for In Situ Ion Substitution and Separation of Salicylic Acid from its Sodium Salt

An electrochemical membrane process (EMP) with three compartments (anolyte, catholyte, and central compartment) based on in-house-prepared cation-exchange membrane (CEM) was developed to achieve in situ ion substitution and recovery of salicylic acid (SAH) from its sodium salt. The physicochemical and electrochemical properties of the ion-exchange membrane (cation- and anion-exchange membrane) under standard operating conditions reveal its suitability for the proposed reactor. Experiments using sodium salicylate (SANa) solutions of different concentrations were carried out under varied applied current density to study the feasibility of the process. Overall electrochemical reaction for the in situ ion substitution and separation of SAH from SANa under operating conditions is also proposed. Results showed that developed EMP with CEMs proved promising for the in situ ion substitution and separation of SAH with recovery of SAH with current efficiency close to 90% and energy consumption around 10 kW h/kg of t...

SPECTROFLUORIMETRIC DETERMINATION OF ACETYLSALICYLIC ACID AND CODEINE MIXTURES IN PHARMACEUTICALS

Acetylsalicylic acid (ASA) and Codeine (CO) are two active ingredients usually found together in pharmaceutical preparations. A lot of procedures for determination of ASA are based on its previous hydrolysis to salicylic acid (SA). In this paper a procedure for both direct determination of CO and indirect determination of ASA in pharmaceuticals is proposed based on the measurements of the native fluorescence of CO and SA (obtained from hydrolysis of ASA). SA was determined in the range 0.1 -1.5 mg/L in the presence up to 10 mg/L of CO at λem 405 nm (λexc = 297nm). CO could not be determined at the low ratio usually found in pharmaceuticals with respect to ASA due to the spectral overlap, so a previous separation of SA was carried out by retention of this on an anion exchange resin. Thus CO was determined in the range 0.1-3 mg/L (λexc=215 nm, λem=350 nm.) in the presence of at least 520 mg/ L of ASA. The procedures were applied to the determination of CO and ASA in commercial pharmaceuticals with goods results, using an HPLC procedure as a reference method.

The determination of slicylic acid and its metabolites in blood plasma by high-performance liquid chromatography with amperometric detection

The separation of salicylic acid and its main metabolites, salicyluric and gentisic acids, by reversed-phase liquid chromatography is followed by electrochemical oxidation in a thin-layer detection cell with a low-temperature isotropic carbon working electrode. The limits of detection for salicylic and gentisic acids are in the subanogram range with linear responses of 0.5–150 ng, 2–250 ng and 0.2–200 ng for salicylic acid, salicyluric acid, and gentisic acid, respectively. The method makes it possible to quantify salicylates simultaneously in human blood plasma.

Determination of traces of salicylic acid in acetylsalicylic acid bulk, tablets and other preparations containing phenacetin and caffeine; Simultaneous determination of salicylic acid, and acetylsalicylic acid with additional components in pharmaceutical preparations

A GLC method for the determination of traces of salicylic acid in acetylsalicylic acid bulk, tablets and other preparations containing phenacetin and caffeine after methylation with methyl iodide and potassium carbonate on a column of 3 % OV-17 on Varaport 30, 70–80 mesh, AW/DMCS is reported. A column-chromatographic separation of salicylic acid from acetylsalicylic acid is necessary prior to methylation on account of the slight hydrolysis of the latter. A ferric chloride-urea reagent holds the salicylic acid back on a Celite 545 column. Further, salicylic acid, acetylsalicylic acid, phenacetin, caffeine, barbital, phenobarbital, bromodiethylacetylcarbamide and codein could also be determined simultaneously through GLC using this methylation technique. The chromatogram of such a mixture is presented.

Separation of salicylic acid, chinophen and aminopyrine by ion-exchange chromatography.

解熱鎮痛剤であるサリチル酸,キノフェンおよびアミノピリンを,イオン交換クロマトグラフ的に分離する方法を検討した.pH4.6に緩衝化したAmberlite CG-50(TypeII)のカラム(9×200～250mm)に,混合試料(各成分1～2mg)を通じたのち,エタノール10vol%を含むpH4.6の酢酸緩衝液を通じると,サリチル酸,キノフェンの順に溶出される.キノフェンの溶離が終わったころ,希塩酸(0.1～1N)に切り替えるとアミノピリンが溶出される.定量は各成分の溶離液について,サリチル酸は波長295mμ,キノフェンは255mμ,アミノピリンは250mμで吸光度を測定し,検量線より求めた.回収率は3成分とも平均95%以上であった.

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