研究目的
To develop an alternative green method for the quantification of sulphamethoxazole and trimethoprim in pharmaceutical formulations using diffuse reflectance infrared spectroscopy and spectral region selection with multivariate calibration.
研究成果
The developed DRIFTS method combined with siPLS algorithm provides a simple, solvent-free, and reliable approach for simultaneous quantification of SMZ and TMP in pharmaceutical tablets, with results within pharmacopoeial limits (93-107%). It offers advantages over traditional HPLC in terms of speed and environmental friendliness, and the spectral region selection improves predictive accuracy.
研究不足
The method may be affected by variations in excipient types and amounts across different manufacturers, potentially requiring a universal calibration set. The study focused on solid dosage forms and specific concentration ranges, which may limit applicability to other formulations or analytes. The need for spectral preprocessing and algorithm optimization could add complexity.
1：Experimental Design and Method Selection:
The study used diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS) combined with partial least squares (PLS) regression. Interval PLS (iPLS) and synergy PLS (siPLS) algorithms were applied to select optimal spectral ranges for quantification, comparing them to full-spectrum PLS models.
2：Sample Selection and Data Sources:
Fifteen commercial tablet formulations and forty-nine synthetic samples were prepared, with concentration ranges of 400-900 mg g-1 for SMZ and 80-240 mg g-1 for TMP. Synthetic samples included excipients like starch and magnesium stearate.
3：List of Experimental Equipment and Materials:
A Nicolet Magna 550 spectrometer with an EasiDiff diffuse reflectance accessory, Spex Certiprep cryogenic mill (model 6750 Freezer Mill), HPLC system (Agilent 1100 Series), and software including Matlab, PLS Toolbox, iToolbox, and Pirouette. Materials included SMZ and TMP bulk drugs, excipients, and HPLC-grade solvents.
4：Experimental Procedures and Operational Workflow:
Samples were ground to particle sizes <80 μm using a cryogenic mill. DRIFTS spectra were recorded from 4000 to 600 cm-1 with 16 scans and 4 cm-1 resolution, using
5：0 ± 3 mg of sample without KBr dilution. Spectral data were preprocessed with multiplicative scatter correction (MSC) and mean centering. HPLC was used as a reference method for validation. Data Analysis Methods:
PLS, iPLS, and siPLS were used for multivariate calibration. Root mean square error of prediction (RMSEP) and cross-validation (RMSECV) were calculated to evaluate model performance. Statistical tests (F-test, t-test) were applied to assess significance.
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