Basavaiah Kanakapura, Anil Kumar Urdigere Rangachar, Tharpa Kalsang
Department of Chemistry, University of Mysore, Manasagangotri Mysore-570 006, India.
Acta Pharm. 2008 Sep;58(3):347-56. doi: 10.2478/v10007-008-0018-z.
A rapid, sensitive and selective method for the determination of raloxifene hydrochloride (RLX) in pure drug and in tablets was developed using gradient high performance liquid chromatography (HPLC). The devised method involved separation of RLX on a reversed phase Hypersil ODS column and determination with UV detection at 284 nm. The standard curve was linear (R = 0.999) over the concentration range of 50-600 microg mL-1 with a detection limit of 0.04 microg mL-1 and a quantification limit of 0.16 microg mL-1. Intra-day and inter-day precision and accuracy of the method were established according to the current ICH guidelines. Intra-day RSD values at three QC levels (250, 450 and 550 microg mL-1) were 0.2-0.5%, based on the peak area. The intra-day relative error (er) was between 0.2 and 0.5%. The developed method was successfully applied to the determination of RLX in tablets and the results were statistically compared with those obtained by a literature method. Accuracy, evaluated by means of the spike recovery method, was the excellent with percent recovery in the range 97.7-103.2 with precision in the range 1.6-2.2%. No interference was observed from the co-formulated substances. The method was economical in terms of the time taken and the amount of solvent used.
采用梯度高效液相色谱法（HPLC）建立了一种快速、灵敏且具选择性的方法，用于测定原料药及片剂中的盐酸雷洛昔芬（RLX）。所设计的方法是在反相Hypersil ODS柱上分离RLX，并于284 nm处采用紫外检测进行测定。标准曲线在50 - 600 μg mL-1浓度范围内呈线性（R = 0.999），检测限为0.04 μg mL-1，定量限为0.16 μg mL-1。该方法的日内和日间精密度及准确度依据现行国际人用药品注册技术协调会（ICH）指南确定。基于峰面积，三个质量控制水平（250、450和550 μg mL-1）的日内相对标准偏差（RSD）值为0.2 - 0.5%。日内相对误差（er）在0.2%至0.5%之间。所建立的方法成功应用于片剂中RLX的测定，并将结果与文献方法所得结果进行了统计学比较。通过加标回收率法评估的准确度极佳，表示回收率在97.7 - 103.2%范围内，精密度在1.6 - 2.2%范围内。未观察到来自共同制剂成分的干扰。该方法在时间消耗和溶剂用量方面较为经济。
