Gumustas Mehmet, Sengel-Turk Ceyda Tuba, Hascicek Canan, Ozkan Sibel A
Ankara University, Faculty of Pharmacy, Department of Analytical Chemistry, Ankara, Turkey.
Biomed Chromatogr. 2014 Oct;28(10):1409-17. doi: 10.1002/bmc.3183. Epub 2014 May 27.
Fulvestrant is used for the treatment of hormone receptor-positive metastatic breast cancer in postmenopausal women with disease progression following anti-estrogen therapy. Several reversed-phase columns with variable silica materials, diameters, lengths, etc., were tested for the optimization study. A good chromatographic separation was achieved using a Waters X-Terra RP(18) column (250 × 4.6 mm i.d. × 5 µm) and a mobile phase, consisting of a mixture of acetonitrile-water (65:35; v/v) containing phosphoric acid (0.1%). The separation was carried out 40 °C with detection at 215 nm.The calibration curves were linear over the concentration range between 1.0-300 and 1.0-200 µg/mL for standard solutions and biological media, respectively. The proposed method is accurate and reproducible. Forced degradation studies were also realized. This fully validated method allows the direct determination of fulvestrant in dosage form and biological samples. The average recovery of the added fulvestrant amount in the samples was between 98.22 and 104.03%. The proposed method was also applied for the determination of fulvestrant from the polymeric-based nanoparticle systems. No interference from using polymers and other excipients was observed in in vitro drug release studies. Therefore an incorporation efficiency of fulvestrant-loaded nanoparticle could be determined accurately and specifically.
氟维司群用于治疗绝经后女性激素受体阳性转移性乳腺癌，这些患者在接受抗雌激素治疗后病情进展。为了进行优化研究，测试了几种具有不同硅胶材料、直径、长度等的反相柱。使用沃特世X-Terra RP(18)柱（250×4.6 mm内径×5 µm）和流动相实现了良好的色谱分离，流动相由含0.1%磷酸的乙腈-水（65:35；v/v）混合物组成。分离在40℃下进行，检测波长为215 nm。标准溶液和生物介质的校准曲线分别在1.0 - 300和1.0 - 200 µg/mL的浓度范围内呈线性。所提出方法准确且可重复。还进行了强制降解研究。这种经过充分验证的方法可直接测定剂型和生物样品中的氟维司群。样品中添加的氟维司群量的平均回收率在98.22%至104.03%之间。所提出的方法还用于测定基于聚合物的纳米颗粒系统中的氟维司群。在体外药物释放研究中未观察到聚合物和其他辅料的干扰。因此，可以准确、特异性地测定载氟维司群纳米颗粒的包封率。
