Czaja Tomasz, Mazurek Sylwester, Szostak Roman
Department of Chemistry, University of Wrocław, 14 F. Joliot-Curie, 50-383 Wrocław, Poland.
Department of Chemistry, University of Wrocław, 14 F. Joliot-Curie, 50-383 Wrocław, Poland.
Talanta. 2016 Dec 1;161:655-659. doi: 10.1016/j.talanta.2016.09.028. Epub 2016 Sep 11.
Diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) is a fast, reliable and cost effective analytical method, requiring minimal or no sample preparation. It is commonly used in the course of qualitative and quantitative analysis of pharmaceutical ingredients and food. We demonstrate that simpler and cheaper specular reflectance (SR) accessory working in a DRIFTS like mode (SR-DL) can be an alternative for DIRFTS attachment. An application of a modified SR accessory for quantitative analysis of solids samples is presented. As a case study the concentration of cinnarizine in commercial tablets has been determined from DRIFTS and SR-DL infrared (IR) and near-infrared (NIR) spectra recorded using DTGS (deuterated triglicine sulphate) detector in the IR and NIR regions and InGaAs (indium-gallium arsenide) detector in the NIR range. Based on these spectra Partial Least Squares (PLS) models were constructed and relative standard errors of prediction (RSEP) were calculated for the calibration, validation and analysed data sets. They amounted to 2.4-2.5%, 2.1-2.7% and 2.0-2.6% for the DRIFTS attachment while 2.1-2.2%, 2.0-2.3% and 1.9-2.6%, respectively, for the modified SR accessory. Obtained error values indicate that modified SR accessory can be effectively used for quantification of solid pharmaceutical samples in the mid- and near-infrared regions.
漫反射傅里叶变换红外光谱法（DRIFTS）是一种快速、可靠且经济高效的分析方法，所需样品制备极少或无需样品制备。它常用于药物成分和食品的定性和定量分析过程中。我们证明，在类似DRIFTS模式下工作的更简单、更便宜的镜面反射（SR）附件（SR-DL）可替代DRIFTS附件。本文介绍了一种改进的SR附件在固体样品定量分析中的应用。作为案例研究，使用DTGS（氘代硫酸三甘肽）探测器在红外和近红外区域以及InGaAs（铟镓砷）探测器在近红外范围内记录的DRIFTS和SR-DL红外（IR）及近红外（NIR）光谱，测定了市售片剂中桂利嗪的浓度。基于这些光谱构建了偏最小二乘法（PLS）模型，并计算了校准、验证和分析数据集的预测相对标准误差（RSEP）。对于DRIFTS附件，这些误差分别为2.4 - 2.5%、2.1 - 2.7%和2.0 - 2.6%，而对于改进的SR附件，误差分别为2.1 - 2.2%、2.0 - 2.3%和1.9 - 2.6%。获得的误差值表明，改进的SR附件可有效用于中红外和近红外区域固体药物样品的定量分析。
