Peris-Vicente Juan, Carda-Broch Samuel, Esteve-Romero Josep
Dep. de Química Física i Analítica, E.S.T.C.E., Universitat Jaume I.
Anal Sci. 2014;30(9):925-30. doi: 10.2116/analsci.30.925.
This paper describes a micellar liquid chromatographic method used to analyze tamoxifen (TAMO) in pharmaceutical formulations, while focusing in its interesting features. Solid samples were solved in a micellar solution, irradiated at 254 nm, filtered and injected. Extraction steps were avoided and thus expediting the procedure. Tamoxifen was resolved in <5 min, using a mobile phase containing 0.15 M sodium dodecyl sulfate-7% pentanol at pH 3, running at 1.5 mL/min under an isocratic mode at 40°C through a C18 column. Detection was achieved by fluorescence by excitation at 260 nm and emission at 380 nm. The validation was performed following the requirements of the International Conference on Harmonization (ICH) Tripartite Guidelines in terms of: specificity, sensitivity, calibration range (0.2 - 20 mg/L), accuracy (98.8 - 101.7%), precision (<1.5%) and robustness (<6.2%). The method was applied to quantify TAMO in TAMO citrate tablets supplied in Spain, and was found appropriate for the quality control of TAMO formulations.
本文介绍了一种用于分析药物制剂中他莫昔芬（TAMO）的胶束液相色谱法，并重点阐述了其有趣的特性。固体样品溶解于胶束溶液中，在254 nm波长下进行照射，过滤后进样。避免了萃取步骤，从而加快了分析过程。使用含0.15 M十二烷基硫酸钠-7%戊醇、pH值为3的流动相，在40°C等度模式下以1.5 mL/min的流速通过C18色谱柱，他莫昔芬在<5分钟内实现分离。通过在260 nm激发波长和380 nm发射波长下的荧光检测来实现测定。按照国际协调会议（ICH）三方指南的要求进行了方法验证，验证内容包括：特异性、灵敏度、校准范围（0.2 - 20 mg/L）、准确度（98.8 - 101.7%）、精密度（<1.5%）和稳健性（<6.2%）。该方法用于对西班牙供应的枸橼酸他莫昔芬片剂中的TAMO进行定量分析，结果表明该方法适用于他莫昔芬制剂的质量控制。
