Attenuated total reflectance with Fourier transform infrared spectroscopy (ATR/FTIR) and different PLS Algorithms for simultaneous determination of clavulanic acid and amoxicillin in powder pharmaceutical formulation

Abstract

Um método para determinação simultânea de ácido clavulânico (CA) e amoxicilina (AMO) foi desenvolvido utilizando a técnica de espectroscopia no infravermelho médio com transformada de Fourier acoplada ao acessório de reflexão total atenuada (ATR/FTIR). Utilizaram-se 27 e 8 amostras para os conjuntos de calibração e previsão, respectivamente. Os modelos de calibração foram desenvolvidos utilizando os algoritmos por mínimos quadrados parciais (PLS), PLS por intervalo (iPLS), PLS por sinergismo (siPLS) e PLS por exclusão (biPLS). Os melhores modelos foram aqueles que utilizaram o algoritmo biPLS. Obtiveram-se erro padrão relativo de previsão (RSEP) de 3,8 e 5,1% para CA e AMO, respectivamente. Os resultados obtidos pela metodologia proposta foram comparados com os obtidos por cromatografia líquida de alta eficiência (HPLC) e nenhuma diferença significativa foi observada. O método proposto utilizando ATR/FTIR associado a métodos de análise multivariados foi satisfatório para determinação de CA e AMO em produtos farmacêuticos.A method for simultaneous determination of clavulanic acid (CA) and amoxicillin (AMO) was developed using Fourier transform mid infrared technique coupled with attenuated total reflectance (ATR/FTIR) accessory. 27 samples were used as calibration set and 8 samples were used for prediction set. Calibration models were developed using partial least squares (PLS), interval PLS (iPLS), synergy PLS (siPLS) and backward PLS (biPLS). Multiplicative scatter correction and the mean centering were used and produced the best models. Relative standard error of prediction (RSEP) of 3.8% for CA and 5.1% for AMO were obtained using biPLS algorithm for ATR/FTIR data. Results obtained by the proposed methodology were compared with those using high performance liquid chromatography (HPLC) and no significant differences were obtained. The proposed method using ATR/FTIR combined to multivariate analysis methods was suitable for the simultaneous determination of CA and AMO in commercial pharmaceutical products.

Rapid Determination of Total Polar Compounds in Frying Oil Using ATR‐FTIR Combined with Extended Partial Least Squares Regression

“…The RMSECV was used to select the optimum number of LVs. [ 38,39 ] The RPD is the ratio of the standard deviation of the reference data in the validation set to the RMSEP; the higher the RPD, the better the model performs. [ 35 ] Generally, an RPD value higher than 3.0 indicates excellent prediction accuracy for analysis, and an RPD between 2.5 and 3.0 implies that the model is precise.…”

Single‐run capillary electrophoresis method for the fast simultaneous determination of amoxicillin, clavulanate, and potassium

“…Several analytical techniques have been applied for AMX and CLA determination in pharmaceutical and biological Abbreviations: AMX, amoxicillin; C 4 samples, such as HPLC [3][4][5][6], TLC with densitometric detection [7], UHPLC-MS/MS [8], CE with UV detection [9,10], MS [11], spectrophotometry [12,13], chemiluminescence [14], attenuated total reflectance with FTIR spectroscopy [15], sequential injection analysis [16][17][18], FIA [19], and stopped-flow techniques [20,21]. Most of the reported methods generally require expensive instrumentation and are time-consuming, which is undesirable in quality control activities.…”

Iodine value determination of edible oils using ATR‐FTIR and chemometric methods

“…Interval partial least-squares (iPLS), proposed by Nørgaard et al for interval selection, represents an approach for local regression modeling of spectral data [17]. Some extended algorithms of iPLS, such as forward iPLS (fiPLS) and backward iPLS (biPLS), have been developed and successfully applied [18][19][20]. However, iPLS, fiPLS, and biPLS have not been used in the determination of IV in fats and oils using FTIR data.…”