经9-芴甲氧羰基柱前衍生化后，采用高效液相色谱-荧光检测法灵敏测定加标人血浆中的曲美他嗪。
Sensitive determination of trimetazidine in spiked human plasma by HPLC with fluorescence detection after pre-column derivatization with 9-fluorenylmethyl chloroformate.
作者信息
Khedr Alaa, Sheha Mahmoud M, Darwish Ibrahim A
机构信息
Pharmaceutical Chemistry Department, Faculty of Pharmacy, King Abdulaziz University, Jeddah, Saudi Arabia.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Sep 1;856(1-2):337-42. doi: 10.1016/j.jchromb.2007.06.036. Epub 2007 Jul 6.
A high-performance liquid chromatographic method for the determination of trimetazidine dihydrochloride (TMZ) in spiked human plasma is described. The method is based on the pre-column derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) using the fluorimetric detection technique. Fluoxetine HCl (FLX) was used as internal standard. Both, TMZ and FLX were completely derivatized after heating at 50 degrees C for 20 min in borate buffer pH 8.0. Samples were analyzed by high performance liquid chromatography (HPLC) using Zorbax-TMS column (250 mm x 4.6 mm, i.d., 5 microm) and mobile phase consist of acetonitrile, methanol and 20 mM sodium acetate pH 4.7 (44:6:50; v/v/v). Fluorescence detector (FLD) was adjusted at excitation and emission wavelengths; 265 and 311 nm, respectively. The linearity of the method was in the range of 4.5-200 ng/ml. Limits of detection (LOD) and quantification (LOQ) were 1.5 and 4.5 ng/ml, respectively. Trimetazidine recovery was 96.5+/-1.3% (n=6; RSD=2.1%).
描述了一种用于测定加标人血浆中盐酸曲美他嗪（TMZ）的高效液相色谱法。该方法基于使用荧光检测技术，用9-芴基甲基氯甲酸酯（FMOC-Cl）进行柱前衍生化。盐酸氟西汀（FLX）用作内标。TMZ和FLX在pH 8.0的硼酸盐缓冲液中于50℃加热20分钟后均完全衍生化。使用Zorbax-TMS柱（250 mm×4.6 mm，内径，5μm）通过高效液相色谱（HPLC）分析样品，流动相由乙腈、甲醇和20 mM pH 4.7的醋酸钠（44:6:50；v/v/v）组成。荧光检测器（FLD）分别在激发和发射波长265和311 nm处进行调节。该方法的线性范围为4.5 - 200 ng/ml。检测限（LOD）和定量限（LOQ）分别为1.5和4.5 ng/ml。曲美他嗪的回收率为96.5±1.3%（n = 6；相对标准偏差=2.1%）。
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