Development and substantiation of a liquid chromatographic method for monitoring organic reactions involved in synthesis of 4-methoxyphenylacetic acid.
A simple and rapid reversed-phase high-performance liquid chromatographic method for monitoring the reactions involved in two different processes for the production of 4-methoxyphenylacetic acid (PMPA) was developed. Impurity profiles of PMPA were used for fingerprinting of the two different synthetic processes by HPLC. Impurities were separated and determined on a Hypersil C18 column with acetonitrile-0.1 M potassium dihydrogen orthophosphate-triethylamine (40:59.95:0.05, v/v) (pH 3.0) as the mobile phase and detection at 280 nm at ambient temperature. The method was substantiated with respect to accuracy, precision, linearity, robustness, limit of detection and quantification. The method was found to be suitable not only for monitoring the reactions but also for quality assurance of PMPA as it could detect impurities at the level of 4 x 10(-9) g.
Rao
R Nageswara
RN
Division of Analytical Chemistry, Indian Institute of Chemical Technology, Tarnaka, Hyderabad. rnrao@iict.ap.nic.in
Nagaraju
D
D
Parimala
P
P
Adapa
Srinivasa R
SR
Alam
M Mujahid
MM
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D010648:Phenylacetates / Q000032:analysis* / Q000138:chemical synthesis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D010648:Phenylacetates; C025136:phenylacetic acid