Ramirez J L, Bellamy M K, Romañac R J
University of Puerto Rico-Mayaguez, Department of Chemistry; PO Box 9019 Mayaguez, Puerto Rico.
AAPS PharmSciTech. 2001 Jul 12;2(3):E11. doi: 10.1208/pt020311.
A near-infrared (NIR) spectroscopic method to determine content uniformity of a large, thick tablet using an approach that could facilitate future validations has been developed. A CT ibuprofen 800-mg tablet weighs about 1150 mg and is about 18.6 mm wide and 7.6 mm thick. The FT NIR spectrometer was optimized for transmission spectra of the tablets by moving it to the sample compartment and placing it immediately behind the tablet. In spite of this dedicated setup, the transmission spectra obtained were very poor, indicating that the NIR radiation was not reaching the detector. The spectra of the tablet improved with use of a simple preparation in which a flat-face die applies pressure of 20 000 psi to the tablet; this reduced the thickness of the tablet from 7.6 mm to 3.6 mm. A calibration model was developed for tablets with drug content ranging from 70% to 130% of label. The calibration model was tested using a validation set of tablets with a drug content of 752, 800, and 848 mg. The results obtained were within 1.5% of the known drug content of the validation set tablets. Even with the sample preparation, the content uniformity results of 10 tablets could be determined using this method in less than 1 hour. The approach described in this article could also be used to validate NIR content uniformity methods for other formulations.
已开发出一种近红外（NIR）光谱法，该方法采用了一种有助于未来验证的方法来测定大型厚片的含量均匀度。一种CT布洛芬800毫克片剂重约1150毫克，宽约18.6毫米，厚约7.6毫米。通过将傅里叶变换近红外光谱仪移至样品室并直接放置在片剂后方，对其进行了优化以获取片剂的透射光谱。尽管采用了这种专门的设置，但获得的透射光谱非常差，这表明近红外辐射未到达检测器。通过一种简单的制备方法改善了片剂的光谱，该方法是使用平面模具对片剂施加20000磅力/平方英寸的压力；这将片剂的厚度从7.6毫米减小到了3.6毫米。针对药物含量在标签量的70%至130%之间的片剂建立了校准模型。使用药物含量为752、800和848毫克的一组验证片剂对校准模型进行了测试。获得的结果在验证集片剂已知药物含量的1.5%以内。即使经过样品制备，使用该方法也可在不到1小时内测定10片片剂的含量均匀度结果。本文所述方法也可用于验证其他制剂的近红外含量均匀度方法。
