Journal of Pharmaceutical and Biomedical Analysis, 2006
In order to evaluate how well existing techniques for transferring NIR calibrations perform for s... more In order to evaluate how well existing techniques for transferring NIR calibrations perform for solid pharmaceutical formulations, a study on four assays of active ingredients was undertaken. The study included two configurations of dispersive NIR instruments and one Fourier transform (FT) instrument. Three methods for calibration transfer: slope/bias correction, local centring and piecewise direct standardisation (PDS), were tested and evaluated. Our conclusions are that the calibration transfer methods tested can perform equally well. It was shown that it is possible to transfer calibrations between instruments of different configurations or even of different types, without loosing the prediction ability of the calibration. To achieve a good calibration transfer, a larger variation in the content of the active ingredient in the samples and more samples are needed for the slope and bias correction method compared to the local centring method. For PDS to be a successful calibration transfer method, an optimisation of the number of transfer samples and how they are selected together with various factors specific for this method is needed. Local centring is the preferred transfer method as its performance is excellent yet it is simple to perform, no optimisation is needed, only a few transfer samples are required and the transfer samples do not have to vary in their content of the active ingredient.
Chemometrics and Intelligent Laboratory Systems, 2003
Near infrared (NIR) transmission spectroscopy is a promising method for fast quantitative measure... more Near infrared (NIR) transmission spectroscopy is a promising method for fast quantitative measurements on pharmaceutical tablets, but there are still some problems to overcome in order to incorporate the technique as a control tool in tablet production. The main problem is the limited precision for multivariate calibrations based on NIR transmission data. The precision is affected by several factors, where one of the most important is which variable to include in the multivariate calibration model.
Transmission geometry is becoming an alternative to the conven-tional re ectance geometry in near... more Transmission geometry is becoming an alternative to the conven-tional re ectance geometry in near-infrared (NIR) spectroscopy of pharmaceuticals. An advantage of transmission NIR is that it sam-ples a volume whereas re ectance NIR merely samples the surface region of ...
Quantitative analysis of pharmaceutical formulations using the new approach of transmission Raman... more Quantitative analysis of pharmaceutical formulations using the new approach of transmission Raman spectroscopy has been investigated. For comparison, measurements were also made in conventional backscatter mode. The experimental setup consisted of a Raman probe-based spectrometer with 785 nm excitation for measurements in backscatter mode. In transmission mode the same system was used to detect the Raman scattered light, while an external diode laser of the same type was used as excitation source. Quantitative partial least squares models were developed for both measurement modes. The results for tablets show that the prediction error for an independent test set was lower for the transmission measurements with a relative root mean square error of about 2.2% as compared with 2.9% for the backscatter mode. Furthermore, the models were simpler in the transmission case, for which only a single partial least squares (PLS) component was required to explain the variation. The main reason for the improvement using the transmission mode is a more representative sampling of the tablets compared with the backscatter mode. Capsules containing mixtures of pharmaceutical powders were also assessed by transmission only. The quantitative results for the capsules' contents were good, with a prediction error of 3.6% w/w for an independent test set. The advantage of transmission Raman over backscatter Raman spectroscopy has been demonstrated for quantitative analysis of pharmaceutical formulations, and the prospects for reliable, lean calibrations for pharmaceutical analysis is discussed.
Time-resolved spectroscopy in the visible and near-infrared (NIR) regions was used in a feasibili... more Time-resolved spectroscopy in the visible and near-infrared (NIR) regions was used in a feasibility study for analysis of solid phar-maceuticals. The objective of the experiments was to study the in-teraction of light with pharmaceutical solids and to investigate the usefulness of the ...
Commercial pressure and patient needs are drivers for reducing the development time for pharmaceu... more Commercial pressure and patient needs are drivers for reducing the development time for pharmaceuticals to market. This leads to increased demands also on pharmaceutical analysis that can no longer afford to rely solely on traditional measurement strategies that may require days for ...
Journal of Pharmaceutical and Biomedical Analysis, 2005
A key issue in near infrared spectroscopy (NIR) is the possibility to use calibrations generated ... more A key issue in near infrared spectroscopy (NIR) is the possibility to use calibrations generated on one instrument for predictions on others. A number of methods for calibration transfer have been proposed, but which method to choose is typically not straightforward. An evaluation of a number of methods for transferring quantitative calibrations between different instruments was carried out on near infrared diffuse-reflectance data from a pharmaceutical formulation. Six instruments were included in the study, five of which were scanning grating instruments, both with and without fibre-optic probe configuration, and one of which was a Fourier-transform instrument, equipped with a fibre-optic probe. The results show that it is possible to transfer calibrations between different instruments, provided that a structured procedure is used. Simple techniques for calibration transfer, such as slope/bias correction on the predicted results, as well as standard normal variate transformation and local centring of the raw spectra, gave considerably lower prediction errors on transfer than did standardisation with a certified diffuse-reflectance standard, or direct transfer without any transfer function. Notably, including more than one instrument in the calibration also improved the prediction ability of the models on calibration transfer. No significant differences in wavelength scale were found when a certified diffuse-reflectance wavelength standard was measured on the instruments studied. Nor did simulated wavelength scale differences below +/-0.3 nm cause any significant change in the prediction errors.
Journal of Pharmaceutical and Biomedical Analysis, 2006
In order to evaluate how well existing techniques for transferring NIR calibrations perform for s... more In order to evaluate how well existing techniques for transferring NIR calibrations perform for solid pharmaceutical formulations, a study on four assays of active ingredients was undertaken. The study included two configurations of dispersive NIR instruments and one Fourier transform (FT) instrument. Three methods for calibration transfer: slope/bias correction, local centring and piecewise direct standardisation (PDS), were tested and evaluated. Our conclusions are that the calibration transfer methods tested can perform equally well. It was shown that it is possible to transfer calibrations between instruments of different configurations or even of different types, without loosing the prediction ability of the calibration. To achieve a good calibration transfer, a larger variation in the content of the active ingredient in the samples and more samples are needed for the slope and bias correction method compared to the local centring method. For PDS to be a successful calibration transfer method, an optimisation of the number of transfer samples and how they are selected together with various factors specific for this method is needed. Local centring is the preferred transfer method as its performance is excellent yet it is simple to perform, no optimisation is needed, only a few transfer samples are required and the transfer samples do not have to vary in their content of the active ingredient.
Chemometrics and Intelligent Laboratory Systems, 2003
Near infrared (NIR) transmission spectroscopy is a promising method for fast quantitative measure... more Near infrared (NIR) transmission spectroscopy is a promising method for fast quantitative measurements on pharmaceutical tablets, but there are still some problems to overcome in order to incorporate the technique as a control tool in tablet production. The main problem is the limited precision for multivariate calibrations based on NIR transmission data. The precision is affected by several factors, where one of the most important is which variable to include in the multivariate calibration model.
Transmission geometry is becoming an alternative to the conven-tional re ectance geometry in near... more Transmission geometry is becoming an alternative to the conven-tional re ectance geometry in near-infrared (NIR) spectroscopy of pharmaceuticals. An advantage of transmission NIR is that it sam-ples a volume whereas re ectance NIR merely samples the surface region of ...
Quantitative analysis of pharmaceutical formulations using the new approach of transmission Raman... more Quantitative analysis of pharmaceutical formulations using the new approach of transmission Raman spectroscopy has been investigated. For comparison, measurements were also made in conventional backscatter mode. The experimental setup consisted of a Raman probe-based spectrometer with 785 nm excitation for measurements in backscatter mode. In transmission mode the same system was used to detect the Raman scattered light, while an external diode laser of the same type was used as excitation source. Quantitative partial least squares models were developed for both measurement modes. The results for tablets show that the prediction error for an independent test set was lower for the transmission measurements with a relative root mean square error of about 2.2% as compared with 2.9% for the backscatter mode. Furthermore, the models were simpler in the transmission case, for which only a single partial least squares (PLS) component was required to explain the variation. The main reason for the improvement using the transmission mode is a more representative sampling of the tablets compared with the backscatter mode. Capsules containing mixtures of pharmaceutical powders were also assessed by transmission only. The quantitative results for the capsules' contents were good, with a prediction error of 3.6% w/w for an independent test set. The advantage of transmission Raman over backscatter Raman spectroscopy has been demonstrated for quantitative analysis of pharmaceutical formulations, and the prospects for reliable, lean calibrations for pharmaceutical analysis is discussed.
Time-resolved spectroscopy in the visible and near-infrared (NIR) regions was used in a feasibili... more Time-resolved spectroscopy in the visible and near-infrared (NIR) regions was used in a feasibility study for analysis of solid phar-maceuticals. The objective of the experiments was to study the in-teraction of light with pharmaceutical solids and to investigate the usefulness of the ...
Commercial pressure and patient needs are drivers for reducing the development time for pharmaceu... more Commercial pressure and patient needs are drivers for reducing the development time for pharmaceuticals to market. This leads to increased demands also on pharmaceutical analysis that can no longer afford to rely solely on traditional measurement strategies that may require days for ...
Journal of Pharmaceutical and Biomedical Analysis, 2005
A key issue in near infrared spectroscopy (NIR) is the possibility to use calibrations generated ... more A key issue in near infrared spectroscopy (NIR) is the possibility to use calibrations generated on one instrument for predictions on others. A number of methods for calibration transfer have been proposed, but which method to choose is typically not straightforward. An evaluation of a number of methods for transferring quantitative calibrations between different instruments was carried out on near infrared diffuse-reflectance data from a pharmaceutical formulation. Six instruments were included in the study, five of which were scanning grating instruments, both with and without fibre-optic probe configuration, and one of which was a Fourier-transform instrument, equipped with a fibre-optic probe. The results show that it is possible to transfer calibrations between different instruments, provided that a structured procedure is used. Simple techniques for calibration transfer, such as slope/bias correction on the predicted results, as well as standard normal variate transformation and local centring of the raw spectra, gave considerably lower prediction errors on transfer than did standardisation with a certified diffuse-reflectance standard, or direct transfer without any transfer function. Notably, including more than one instrument in the calibration also improved the prediction ability of the models on calibration transfer. No significant differences in wavelength scale were found when a certified diffuse-reflectance wavelength standard was measured on the instruments studied. Nor did simulated wavelength scale differences below +/-0.3 nm cause any significant change in the prediction errors.
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