使用反射近红外光谱和傅里叶变换拉曼光谱法测定片剂中噻氯匹定的定量无损方法。
Quantitative nondestructive methods for the determination of ticlopidine in tablets using reflectance near-infrared and Fourier transform Raman spectroscopy.
作者信息
Markopoulou C K, Koundourellis J E, Orkoula M G, Kontoyannis C G
机构信息
Laboratory of Pharmaceutical Analysis, School of Pharmacy, Aristotelian University of Thessaloniki, 54124 Thessaloniki, Greece.
出版信息
Appl Spectrosc. 2008 Feb;62(2):251-7. doi: 10.1366/000370208783575636.
Two different nondestructive spectroscopy methods based on near-infrared (NIR) and Fourier transform (FT) Raman spectroscopy were developed for the determination of ticlopidine-hydrochloride (TCL) in pharmaceutical formulations and the results were compared to those obtained by high-performance liquid chromatography (HPLC). An NIR assay was performed by reflectance over the 850-1700 nm region using a partial least squares (PLS) prediction model, while the absolute FT-Raman intensity of TCL's most intense vibration was used for constructing the calibration curve. For both methodologies the spectra were obtained from the as-received film-coated tablets of TCL. The two quantitative techniques were built using five "manual compressed" tablets containing different concentrations and validated by evaluating the calibration model as well as the accuracy and precision. The models were applied to commercial preparations (Ticlid). The results were compared to those obtained from the application of HPLC using the methodology described by "Sanofi Research Department" and were found to be in excellent agreement, proving that NIR, using fiber-optic probes, and FT-Raman spectroscopy can be used for the fast and reliable determination of the major component in pharmaceutical analysis.
开发了两种基于近红外(NIR)和傅里叶变换(FT)拉曼光谱的不同无损光谱方法,用于测定药物制剂中的盐酸噻氯匹定(TCL),并将结果与通过高效液相色谱(HPLC)获得的结果进行比较。通过使用偏最小二乘法(PLS)预测模型在850 - 1700 nm区域进行反射率测定来进行近红外分析,而TCL最强振动的绝对FT - 拉曼强度用于构建校准曲线。对于这两种方法,光谱均从收到的TCL薄膜包衣片剂中获得。这两种定量技术是使用五片含有不同浓度的“手动压制”片剂建立的,并通过评估校准模型以及准确性和精密度进行验证。这些模型应用于商业制剂(抵克立得)。将结果与使用“赛诺菲研究部”描述的方法通过HPLC应用获得的结果进行比较,发现结果非常一致,证明使用光纤探头的近红外和FT - 拉曼光谱可用于药物分析中主要成分的快速可靠测定。