Research Institute of Electronics, Shizuoka University , Hamamatsu, Shizuoka 432-8011, Japan.
Division of Drugs, National Institute of Health Sciences , Setagaya, Tokyo 158-8501, Japan.
Anal Chem. 2018 Feb 6;90(3):1677-1682. doi: 10.1021/acs.analchem.7b03220. Epub 2018 Jan 19.
Quantitative detection of impurities in organic crystals was demonstrated by accurately measuring absorption frequencies using a continuous wave gallium phosphide terahertz spectrometer. THz spectra of l-asparagine monohydrate doped with l-aspartic acid at 0.05 to 12.5 wt % were obtained at 10 K. The three lowest frequency absorption peaks were baseline-resolved, allowing them to be examined independently. Using a least-squares curve fitting technique, impurities were detected at levels as low as 500 ppm. The sensitivity and detection limits of the technique depended strongly on the nature of both the host and the impurities. The projected limit of detection using the current system, given optimal materials, was estimated to be 51.7 ppm. In addition to quantitative assessments, impurities may also be identified by comparing frequency shifts of multiple absorptions.
利用连续波砷化镓太赫兹光谱仪准确测量吸收频率,实现了对有机晶体中杂质的定量检测。在 10 K 下获得了浓度为 0.05 至 12.5wt%的 L-天冬酰胺一水合物掺杂 L-天冬氨酸的太赫兹光谱。通过基线分辨三个最低频率的吸收峰,可以独立地对它们进行研究。使用最小二乘曲线拟合技术,可以检测到低至 500ppm 的杂质。该技术的灵敏度和检测限强烈依赖于主客体和杂质的性质。考虑到最优材料,使用当前系统估计的检测极限约为 51.7ppm。除了定量评估之外,通过比较多个吸收的频率移动,也可以识别杂质。