Abstract
In a short runtime process (about 6 minutes), with isocratic method without need of reconditioning before the next run, a mixture of some molecules containing 4-aminophenol (4APh), phenol, 3-nitrosalicylic acid (3NSA), and mesalamine (5-aminosalicylic acid) (MLZ), were separated and detected by means of HPLC/UV-Vis system. The resolutions of the separated and sharp peaks referring to the mentioned compounds were at least more than 2, and the tailing factor (TF) was about 1, even in 1 µg/l (ppm) concentration. In order to optimize the method, the effects of the pH, eluent percentage, flow rate, and buffer concentration, and wavelength on the chromatogram were investigated. Also, the results of the validation processes showed that the method trustable to be used in laboratories.
Highlights
In one hand, separation and detection of trace amounts of phenolic or benzylic acid compounds are important both in medicinal[1] and environmental chemistry,[2] and in the other hand, determination of one part per million (PPM or μg/l) concentration of some of the aminophenols in Mesalazine is crucial in pharmacology.[3]
In order to find the best chromatography condition with higher possible separation, resolution, and linearity, and to reach to the lowest limit of detection, several parameters containing the concentration of PDP, and octanesulfonic acid sodium salt (OSA) salts, pH of the buffer, organic solvent percentage, flow rate, and wavelength were optimized
The results showed that decreasing the PDP salt in buffer or even elimination of that, could result in better separation and higher resolution of all four peaks
Summary
Separation and detection of trace amounts of phenolic or benzylic acid compounds are important both in medicinal (human metabolism)[1] and environmental chemistry,[2] and in the other hand, determination of one part per million (PPM or μg/l) concentration of some of the aminophenols in Mesalazine is crucial in pharmacology.[3] Due to these requirements, designing suitable methods for Related Impurity Analysis (RIA),[4,5] Assay Analysis (AA),[6] Residual Solvent Analysis (by gas chromatography) (RSA),[7] and other instrumental analysis for MLZ and related compounds were designed, and widely applied. Song and colleagues designed an electrochemical method for RIA of MLZ using a C8 column, with the mobile phase of PDP, and sodium 1-octanesulfonic acid sodium salt (OSA) buffer solution at pH 2.2, methanol, acetonitrile (890:80:30) and methanol via gradient elution.
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