Blanco M, Bautista M, Alcalà M
Departament de Química, Unitat de Química Analítica, Universitat Autònoma de Barcelona, Bellaterra, 08193 Barcelona, Spain.
AAPS PharmSciTech. 2008;9(4):1130-5. doi: 10.1208/s12249-008-9156-3. Epub 2008 Nov 14.
The purpose of this research was to demonstrate the ability of reflectance near-infrared (NIR) spectroscopy for quantitative analysis of an active ingredient in different production steps of a solid formulation. The drug is quantified at two different steps of a pharmaceutical process: after granulation and after tablet coating. Calibration samples were prepared by mixing pure drug, excipients, and batch samples (75-120 mg/g active ingredient) using a simple methodology that can be easily carried out in a laboratory. Partial least squares calibration models were calculated in second-derivative mode using the wavelength range 1,134-1,798 nm. The error of prediction for granulated samples was 1.01% and 1.63% for tablets. The results prove that NIR spectroscopy is a good alternative to other, more time-consuming means of analysis for pharmaceutical process monitoring.
本研究的目的是证明反射近红外（NIR）光谱法对固体制剂不同生产步骤中活性成分进行定量分析的能力。该药物在制药过程的两个不同步骤进行定量：制粒后和包衣后。校准样品通过使用一种简单的方法混合纯药物、辅料和批次样品（75 - 120 mg/g活性成分）制备，该方法可在实验室轻松进行。使用1134 - 1798 nm波长范围以二阶导数模式计算偏最小二乘校准模型。制粒样品的预测误差为1.01%，片剂的预测误差为1.63%。结果证明，近红外光谱法是制药过程监测中其他更耗时分析方法的良好替代方法。
