Koleva Bojidarka B, Kolev Tsonko M, Tsalev Dimiter L, Spiteller Michael
University of Sofia St. Kl. Ohridsky, Faculty of Chemistry, Department of Analytical Chemistry, Sofia 1164, Bulgaria.
J Pharm Biomed Anal. 2008 Jan 22;46(2):267-73. doi: 10.1016/j.jpba.2007.09.022. Epub 2007 Sep 29.
Quantitative infrared (IR) and Raman spectroscopic approach for determination of phenacetin (Phen) and salophen (Salo) in binary solid mixtures with caffeine: phenacetin/caffeine (System 1) and salophen/caffeine (System 2) is presented. Absorbance ratios of 746 cm(-1) or 721 cm(-1) peaks (characteristic for each of determined compounds in the Systems 1 and 2) to 1509 cm(-1) and 1616 cm(-1) (attributed to Phen and Salo, respectively) were used. The IR spectroscopy gives confidence of 98.9% (System 1) and 98.3% (System 2), while the Raman spectroscopic data are with slightly higher confidence of 99.1% for both systems. The limits of detection for the compounds studied were 0.013 and 0.012 mole fraction for IR and Raman methods, respectively. Solid-state linear dichroic infrared (IR-LD) spectral analysis of solid mixtures was carried out with a view to obtaining experimental IR spectroscopic assignment of the characteristic IR bands of both determined compounds. The orientation technique as a nematic liquid crystal suspension was used, combined with the so-called reducing-difference procedure for polarized spectra interpretation. The possibility for obtaining supramolecular stereo structural information for Phen and Salo by comparing spectroscopic and crystallographic data has also been shown. An independent high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis was performed for comparison and validation of vibrational spectroscopy data. Applications to 10 tablets of commercial products APC and Sedalgin are given.
介绍了一种用于测定与咖啡因形成的二元固体混合物中对乙酰氨基酚（Phen）和沙罗芬（Salo）的定量红外（IR）和拉曼光谱方法：对乙酰氨基酚/咖啡因（体系1）和沙罗芬/咖啡因（体系2）。使用746 cm⁻¹或721 cm⁻¹峰（分别为体系1和体系2中每种测定化合物的特征峰）与1509 cm⁻¹和1616 cm⁻¹（分别归因于Phen和Salo）的吸光度比。红外光谱法对体系1的置信度为98.9%，对体系2的置信度为98.3%，而拉曼光谱数据对两个体系的置信度略高，为99.1%。所研究化合物的红外和拉曼方法的检测限分别为0.013和0.012摩尔分数。对固体混合物进行了固态线性二向色红外（IR-LD）光谱分析，以获得两种测定化合物特征红外波段的实验红外光谱归属。使用向列型液晶悬浮液的取向技术，并结合所谓的还原差分程序来解释偏振光谱。通过比较光谱和晶体学数据获得Phen和Salo超分子立体结构信息的可能性也得到了证明。进行了独立的高效液相色谱-串联质谱（HPLC-MS/MS）分析，以比较和验证振动光谱数据。给出了在10片商业产品APC和塞达林上的应用。
