Basavaiah Kanakapura, Tharpa Kalsang, Anil Kumar Urdigere Rangachar, Rajedraprasad Nagaraju, Hiriyanna Salmara ganeshbhat, Vinay Kanakapura Basavaiah
Department of Chemistry, University of Mysore, Manasagangothri, Mysore-570006, India.
Arch Pharm Res. 2009 Sep;32(9):1271-9. doi: 10.1007/s12272-009-1913-7. Epub 2009 Sep 26.
Two simple and sensitive spectrophotometric methods are described for the determination of raloxifene hydrochloride (RLX) in pure form and in tablets. The first method (method A) is based on the formation of a yellowish-brown chromogen peaking at 430 nm when RLX was reacted with permanganate in acetic acid medium. In the second method (method B), RLX was reacted with a measured excess of permanganate in H2SO4 medium followed by the spectrophotometric measurement of the unreacted KMnO4 at 550 nm. Under the optimized experimental conditions, Beer's law is obeyed in the concentration range 0.6-6.0 and 1.5-15.0 microg mL(-1) with molar absorptivity of 7.01 x 10(4) and 2.8 x 10(4) L mol(-1) cm(-1) for method A and method B, respectively. The limits of detection (LOD) and quantification (LOQ) have also been reported. The intra-day and inter-day RSD and RE values at three different concentrations were assessed. The proposed methods were applied to the commercially available tablets, and the results were statistically compared with those of the reference method. The accuracy and reliability of the methods were further ascertained by recovery studies.
本文描述了两种简单且灵敏的分光光度法，用于测定纯品及片剂中的盐酸雷洛昔芬（RLX）。第一种方法（方法A）基于在乙酸介质中，当RLX与高锰酸盐反应时形成一种在430 nm处有吸收峰的黄褐色显色剂。第二种方法（方法B）是在硫酸介质中，使RLX与过量的高锰酸盐反应，然后在550 nm处对未反应的KMnO₄进行分光光度测定。在优化的实验条件下，方法A和方法B在浓度范围分别为0.6 - 6.0和1.5 - 15.0 μg mL⁻¹时符合比尔定律，摩尔吸光系数分别为7.01×10⁴和2.8×10⁴ L mol⁻¹ cm⁻¹。还报道了检测限（LOD）和定量限（LOQ）。评估了三种不同浓度下的日内和日间相对标准偏差（RSD）及相对误差（RE）值。将所提出的方法应用于市售片剂，并将结果与参考方法进行统计学比较。通过回收率研究进一步确定了方法的准确性和可靠性。
