Detection of Drug Active Ingredients by Chemometric Processing of Solid-State NMR Spectrometry Data—The Case of Acetaminophen

Abstract

This paper presents a preliminary study in building discriminant models from solid-state NMR spectrometry data to detect the presence of acetaminophen in over-the-counter pharmaceutical formulations. The dataset, containing 11 spectra of pure substances and 21 spectra of various formulations, was processed by partial least squares discriminant analysis (PLS-DA). The model found coped with the discrimination, and its quality parameters were acceptable. It was found that standard normal variate preprocessing had almost no influence on unsupervised investigation of the dataset. The influence of variable selection with the uninformative variable elimination by PLS method was studied, reducing the dataset from 7601 variables to around 300 informative variables, but not improving the model performance. The results showed the possibility to construct well-working PLS-DA models from such small datasets without a full experimental design.

Characterization of pharmaceutically relevant materials at the solid state employing chemometrics methods

“…Two of these studies, employing XRPD and DSC, respectively, have been developed by the group of Komsta [53,54]. The third set of models was built from ssNMR spectroscopic data, with the aim to detect the presence of acetaminophen in over-the-counter pharmaceutical formulations [55].…”

RP-LC and TLC Densitometric Determination of Paracetamol and Pamabrom in Presence of Hazardous Impurity of Paracetamol and Application to Pharmaceuticals

“…[20][21][22][23] A chemometric technique was also used for the determination of PARA. 24 Few methods have been reported for the simultaneous determination of PARA and PAP, including spectrophotometry, 25 electrochemical determination, 26 and using sequential injection analysis. 27 A literature survey revealed that few methods were reported for the determination of PAMB, including spectrophotometry, 28,29 and HPTLC.…”