Molecularly imprinted polymer (MIP) for sulfanilamide (SN) sensing is prepared through in‐situ electropolymerization of pyrrole (Py) on pencil graphite electrode (PGE). Computational study using density functional theory with B3LYP level is performed to analyze and evaluate the template‐monomer geometry. Among the various functional monomers studied pyrrole is found to have the highest binding interaction energy with SN and it is chosen as a functional monomer. Electropolymerization of pyrrole in the presence of SN on PGE is carried out using cyclic voltammetry. Structural morphology of the imprinted polymer is characterized by field emission scanning electron microscopy (FESEM) studies. Quantitative measurements of MIP based SN detection are performed by using cyclic voltammetry and differential pulse voltammetry studies. Several important kinetic parameters influencing the performance of SN sensor such as limit of detection, linear concentration range and sensitivity etc. are determined and analyzed. Under the optimized conditions, MIP based SN sensor proposed in this work has a very low detection limit of 2.0×10−8 M (S/N=3) and possesses two linear ranges from 5.0×10−8 to 1.1×10−6 M and 1.1×10−6 to 48×10−6 M with a sensitivity value of 1.158 and 0.012 µA/µM respectively. This particular sensor shows a good selectivity towards SN in presence of potential other structural analogue interferences namely sulfamethaxazole, sulfathiazole and sulfadiazine. Furthermore, the fabricated sensor is successfully applied to quantitatively determine and analyze SN present in spiked human serum and ground water samples.
Although a number of methods are available for evaluating Linezolid and its possible impurities, a common method for separation if its potential impurities, degradants and enantiomer in a single method with good efficiency remain unavailable. With the objective of developing an advanced method with shorter runtimes, a simple, precise, accurate stability-indicating LC method was developed for the determination of purity of Linezolid drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. This method is capable of separating all the related substances of Linezolid along with the chiral impurity. This method can also be used for the estimation of assay of Linezolid in drug substance as well as in drug product. The method was developed using Chiralpak IA (250 mm×4.6 mm, 5 μm) column. A mixture of acetonitrile, ethanol, n-butyl amine and trifluoro acetic acid in 96:4:0.10:0.16 (v/v/v/v) ratio was used as a mobile phase. The eluted compounds were monitored at 254 nm. Linezolid was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantification, precision, linearity, accuracy, robustness and system suitability.
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