Belal F, Sharaf El-Din Mohie K, Elenany N, Saad S
Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, 35516, Mansoura, Egypt.
Luminescence. 2014 Sep;29(6):559-65. doi: 10.1002/bio.2577. Epub 2013 Oct 21.
A simple and rapid liquid chromatographic method was developed and validated for the determination of triclabendazole with high accuracy and precision within 6 min. Good chromatographic separation was achieved using a CLC Shim-pack C8 (250 × 4.6 mm, 5 µm particle size) using the mobile phase containing a mixture of 0.02 m phosphate buffer and methanol with a ratio of (20 : 80 v/v) at pH 4.0 was pumped at a flow rate of 1.2 mL/min with fluorescence detection for the first time at 338 nm after excitation at 298 nm. Losartan potassium was used as an internal standard. The method showed good linearity in the ranges of 0.05-2.0 µg/mL with limits of detection and quantification of 14.1 and 42.6 ng/mL, respectively. The suggested method was successfully applied for the analysis of triclabendazole in tablets. The high sensitivity of the method enabled the determination of the studied drug in spiked human plasma with mean percentage of recoveries of 99.79 ± 5.09. Statistical evaluation of the data was performed according to ICH Guidelines.
建立了一种简单快速的液相色谱法，用于在6分钟内高精度、高精准度地测定三氯苯达唑。使用CLC Shim-pack C8（250×4.6 mm，5 µm粒径）色谱柱，以含有0.02 m磷酸盐缓冲液和甲醇的混合液（比例为20:80 v/v）作为流动相，pH为4.0，流速为1.2 mL/min，首次在298 nm激发后于338 nm处进行荧光检测，实现了良好的色谱分离。以氯沙坦钾作为内标。该方法在0.05 - 2.0 µg/mL范围内具有良好的线性，检测限和定量限分别为14.1和42.6 ng/mL。所建议的方法成功应用于片剂中三氯苯达唑的分析。该方法的高灵敏度能够测定加标人血浆中的研究药物，平均回收率为99.79±5.09%。数据的统计评估按照国际人用药品注册技术协调会（ICH）指南进行。
