光谱学与光谱分析, 2017, 37 (1): 120, 网络出版: 2017-02-09
拉曼光谱在多组分定量分析中方法学验证的探讨
The Study of Methodology Validation in Multicomponent Quantitative Analysis of Raman Spectroscopy
方法学验证 拉曼光谱法 多组分定量 数学模型验证与评价 Methodology validation Raman spectroscopy Multicomponent quantitative analysis Mathematical model validation and evaluation
摘要
拉曼光谱在中国药典2010版第一次被收录于“附录XIX L拉曼光谱法指导原则”中, 但该原则对拉曼多组分定量分析的方法学验证未作论述, 对多组分复杂体系中采用拉曼数学模型定量分析时的方法学验证进行独创性的探索和研究, 分别从仪器性能测试、 线性、 定量限、 准确度等方面进行方法学验证研究; 另外由于拉曼光谱定量数学模型样品为复杂成分样品, 无须像传统方法提供空白样品和进行破坏实验等专属性实验验证。 通过研究探讨, 提出了拉曼多组分定量分析的方法学验证内容, 为方法学验证的完善和标准的制定提供了基础和依据。
Abstract
Raman spectroscopy with the help of sophisticated data analysis techniques based on multivariate analysis have made it possible to study the full information of Raman spectra and to draw conclusions about the chemical structure and composition of very complex systems. As Raman spectroscopy has the advantage to provide rich information of the sample, so it was first included in Chinese Pharmacopoeia (2010) as “Annex XIX L Guidelines of Raman spectroscopy”. However the validation method for multicomponent quantitative analysis of Raman spectroscopy was not discussed in this pharmacopoeia. The purpose of this study was to develop innovatively the validation method for the Raman model in multicomponent quantitative analysis. Two kinds of samples with different matrix background were used to study the self-performance test of the instrument, linearity, limit of quantitation, accuracy and precision, respectively. As the sample was complex composition in our study, so there is no need to provide sample blank and rupture test for specificity study which was carried out in the traditional method of experiments. As the result showed, we propose a validation method for Raman spectroscopy in multicomponent analysis for the further study and improvement of standards of the method.
薛金涛, 李春燕, 吴纯洁, 叶利明. 拉曼光谱在多组分定量分析中方法学验证的探讨[J]. 光谱学与光谱分析, 2017, 37(1): 120. XUE Jin-tao, LI Chun-yan, WU Chun-jie, YE Li-ming. The Study of Methodology Validation in Multicomponent Quantitative Analysis of Raman Spectroscopy[J]. Spectroscopy and Spectral Analysis, 2017, 37(1): 120.