Department of Chemistry and Research Institute for Natural Sciences, Hanyang University, Seoul 133-791, Republic of Korea.
J Pharm Biomed Anal. 2010 Nov 2;53(3):762-6. doi: 10.1016/j.jpba.2010.05.008. Epub 2010 May 13.
The concentration of TiO(2) in a cream formulation has been non-destructively measured using Raman spectroscopy without further sample pretreatments. The distribution of TiO(2) particles in a highly viscous cream may not be homogeneous on a microscopic scale and local aggregation of the particles is possible; therefore, acquisition of Raman spectra capable of representing the whole sample identity rather than the localized chemical information was critically necessary to ensure reliable quantitative analysis. A wide area illumination (WAI) scheme, applying 6-mm diameter laser illumination area (total coverage: 28.3mm(2)) on a sample, was used to achieve representative sample presentation and improved accuracy. When Raman spectra were collected for the same sample using a conventional scheme with a much smaller laser spot ( approximately 100 microm), the spectral reproducibility was degraded, as expected. The local aggregation of TiO(2) particles was confirmed by analyzing both SEM (scanning electron microscopy) and Raman images of a cream sample. When the WAI scheme was used, the resulting error in the determination of TiO(2) concentration was 0.03 wt%, while 0.17 wt% in the case of using the conventional scheme. The proposed Raman scheme would be advantageous over the conventional titration method that requires destructive incineration of the organic cream matrix, as well as a large consumption of chemical reagents.
采用 Raman 光谱法,无需进一步的样品预处理,可无损地测量乳膏制剂中 TiO(2)的浓度。在高度粘稠的乳膏中,TiO(2)颗粒的分布在微观尺度上可能不均匀,并且颗粒可能局部聚集;因此,采集能够代表整个样品特征而不是局部化学信息的 Raman 光谱对于确保可靠的定量分析至关重要。使用宽区域照明(WAI)方案,将 6 毫米直径的激光照射区域(总覆盖面积:28.3 毫米²)应用于样品,以实现代表性的样品呈现和提高准确性。当使用具有更小激光光斑(约 100 微米)的常规方案对同一样品采集 Raman 光谱时,光谱重现性如预期的那样降低。通过分析乳膏样品的 SEM(扫描电子显微镜)和 Raman 图像,证实了 TiO(2)颗粒的局部聚集。当使用 WAI 方案时,TiO(2)浓度测定的误差为 0.03wt%,而使用常规方案时为 0.17wt%。与需要破坏性地焚烧有机乳膏基质以及大量消耗化学试剂的传统滴定法相比,建议的 Raman 方案具有优势。