Department of Chemistry, University of Wrocław, Poland.
Drug Test Anal. 2013 Feb;5(2):126-9. doi: 10.1002/dta.379. Epub 2012 Apr 17.
An efficient method for the quantitative determination of acetaminophen (AAP) and diclofenac sodium (DS) in commercial suppositories based on partial least squares (PLS) treatment of FT-Raman spectra is described. The relative standard errors of prediction (RSEP) were calculated for calibration and validation data sets to evaluate the quality of the constructed models. In the case of DS determination, RSEP error values of 1.9 % and 2.3 % for the calibration and validation data sets, respectively, were found. For AAP these errors amounted to 1.6-2.3 % and 1.8-2.8 %, respectively, for the different calibration models. Four commercial preparations containing 5, 12.5, 16.7 and 33.3 % (w/w) AAP and one containing 5 % (w/w) DS were successfully quantified using the developed models. Concentrations derived from the developed models correlated strongly with the declared values and yielded recoveries of 99.4-100.2 % and 99.6 % for AAP and DS, respectively. The proposed procedure can be used as a fast, economic and reliable method for quantification of the active pharmaceutical ingredients in suppositories.
一种基于傅里叶变换拉曼光谱偏最小二乘法（PLS）处理的高效定量测定商业栓剂中对乙酰氨基酚（AAP）和双氯芬酸钠（DS）的方法。通过计算校准和验证数据集的相对预测标准误差（RSEP）来评估所构建模型的质量。在 DS 测定的情况下，校准和验证数据集的 RSEP 误差值分别为 1.9%和 2.3%。对于 AAP，不同校准模型的误差值分别为 1.6-2.3%和 1.8-2.8%。使用所开发的模型成功定量了四种含有 5%、12.5%、16.7%和 33.3%（w/w）AAP 的商业制剂和一种含有 5%（w/w）DS 的制剂。从所开发的模型得出的浓度与宣称值密切相关，AAP 和 DS 的回收率分别为 99.4-100.2%和 99.6%。该方法快速、经济、可靠，可用于栓剂中活性药物成分的定量分析。
