The performance of different chemometric approaches was evaluated in the spectrophotometric determination of pharmaceutical mixtures characterized by having the amount of components with a very high ratio. Principal c...The performance of different chemometric approaches was evaluated in the spectrophotometric determination of pharmaceutical mixtures characterized by having the amount of components with a very high ratio. Principal component regression （PCR）, partial least squares with one dependent variable （PLS1） or multi-dependent variables （PLS2）, and multivariate curve resolution （MCR） were applied to the spectral data of a ternary mixture containing paracetamol, sodium ascorbate and chlorpheniramine （150：140：1, m/m/m）, and a quaternary mixture containing paracetamol, caffeine, phenylephrine and chlorpheniramine （125：6. 25：1.25：1, m/m/m/m）. The UV spectra of the calibration samples in the range of 200-320 nm were pre-treated by removing noise and useless data, and the wavelength regions having the most useful analytical information were selected using the regression coefficients calculated in the multivariate modeling. All the defined chemometric models were validated on external sample sets and then applied to commercial pharmaceutical formulations. Different data intervals, fixed at 0.5, 1.0, and 2.0 point/nm, were tested to optimize the prediction ability of the models. The best results were obtained using the PLSlcalibration models and the quantification of the species of a lower amount was sig- nificantly improved by adopting 0.5 data interval, which showed accuracy between 94.24% and 107.76%.展开更多
A supersaturated design （SSD）, whose run size is not enough for estimating all the main effects, is commonly used in screening experiments. It offers a potential useful tool to investigate a large number of factors ...A supersaturated design （SSD）, whose run size is not enough for estimating all the main effects, is commonly used in screening experiments. It offers a potential useful tool to investigate a large number of factors with only a few experimental runs. The associated analysis methods have been proposed by many authors to identify active effects in situations where only one response is considered. However, there are often situations where two or more responses are observed simultaneously in one screening experiment, and the analysis of SSDs with multiple responses is thus needed. In this paper, we propose a two-stage variable selection strategy, called the multivariate partial least squares-stepwise regression （MPLS-SR） method, which uses the multivariate partial least squares regression in conjunction with the stepwise regression procedure to select true active effects in SSDs with multiple responses. Simulation studies show that the MPLS-SR method performs pretty good and is easy to understand and implement.展开更多
基金Ministero dell'Istruzione,dell'Universitàe della Ricerca(MIUR),Italy,for the financial support to this work,grant 60%2014
文摘The performance of different chemometric approaches was evaluated in the spectrophotometric determination of pharmaceutical mixtures characterized by having the amount of components with a very high ratio. Principal component regression （PCR）, partial least squares with one dependent variable （PLS1） or multi-dependent variables （PLS2）, and multivariate curve resolution （MCR） were applied to the spectral data of a ternary mixture containing paracetamol, sodium ascorbate and chlorpheniramine （150：140：1, m/m/m）, and a quaternary mixture containing paracetamol, caffeine, phenylephrine and chlorpheniramine （125：6. 25：1.25：1, m/m/m/m）. The UV spectra of the calibration samples in the range of 200-320 nm were pre-treated by removing noise and useless data, and the wavelength regions having the most useful analytical information were selected using the regression coefficients calculated in the multivariate modeling. All the defined chemometric models were validated on external sample sets and then applied to commercial pharmaceutical formulations. Different data intervals, fixed at 0.5, 1.0, and 2.0 point/nm, were tested to optimize the prediction ability of the models. The best results were obtained using the PLSlcalibration models and the quantification of the species of a lower amount was sig- nificantly improved by adopting 0.5 data interval, which showed accuracy between 94.24% and 107.76%.
基金supported by the National Natural Science Foundation of China （Grant Nos. 10971107, 11271205）, the ＂131＂ Talents Program of Tianjin, and the Fundamental Research Funds for the Central Universities （Grant Nos. 65030011, 65011481）.
文摘A supersaturated design （SSD）, whose run size is not enough for estimating all the main effects, is commonly used in screening experiments. It offers a potential useful tool to investigate a large number of factors with only a few experimental runs. The associated analysis methods have been proposed by many authors to identify active effects in situations where only one response is considered. However, there are often situations where two or more responses are observed simultaneously in one screening experiment, and the analysis of SSDs with multiple responses is thus needed. In this paper, we propose a two-stage variable selection strategy, called the multivariate partial least squares-stepwise regression （MPLS-SR） method, which uses the multivariate partial least squares regression in conjunction with the stepwise regression procedure to select true active effects in SSDs with multiple responses. Simulation studies show that the MPLS-SR method performs pretty good and is easy to understand and implement.
