Hvattum E, Normann P T, Jamieson G C, Lai J J, Skotland T
Nycomed Imaging AS, Torshov, Oslo, Norway.
J Pharm Biomed Anal. 1995 Jun;13(7):927-32. doi: 10.1016/0731-7085(95)01311-8.
A narrow-bore high-performance liquid chromatography method was developed for simultaneous separation of gadolinium diethylenetriaminepentaacetic acid (GdDTPA), the monomethylamide (GdDTPA-MMA) and the bis-methylamide (GdDTPA-BMA) in human serum and urine. The Gd complexes were detected at 658 nm after post-column derivatization with Arsenazo III. The serum samples were ultrafiltrated, whereas the urine samples were centrifuged and diluted before analysis. With an injection volume of 10 microliters on a 2.1 mm ID reversed-phase column, the limit of detection of GdDTPA-BMA was calculated as 0.3 microM and 1.1 microM in serum and urine, respectively. The method was validated with respect to GdDTPA-BMA with a limit of quantification set to 2 microM and 10 microM in serum and urine, respectively. The best fit of the calibration curve was obtained using non-linear regression according to the equation Y = A+BX+CX2 in the concentration ranges 2-800 microM and 10-2000 microM of GdDTPA-BMA in serum and urine, respectively. The precision of the method was found to range from 1 to 4% RSD. The recoveries of GdDTPA-BMA spiked in serum and urine were higher than 95% with an RSD equal to or less than 4%. The serum samples were stable for at least 5 months when stored at -70 degrees C, and the urine samples were stable for a least 6 months when stored at -20 degrees C.
建立了一种窄孔高效液相色谱法，用于同时分离人血清和尿液中的钆二乙三胺五乙酸（GdDTPA）、单甲酰胺（GdDTPA-MMA）和双甲酰胺（GdDTPA-BMA）。用偶氮胂III进行柱后衍生后，在658nm处检测钆配合物。血清样品进行超滤，而尿液样品在分析前进行离心和稀释。在2.1mm内径的反相柱上进样10微升，GdDTPA-BMA在血清和尿液中的检测限分别计算为0.3 microM和1.1 microM。该方法针对GdDTPA-BMA进行了验证，血清和尿液中的定量限分别设定为2 microM和10 microM。在血清和尿液中GdDTPA-BMA的浓度范围分别为2-800 microM和10-2000 microM时，根据方程Y = A+BX+CX2使用非线性回归获得校准曲线的最佳拟合。发现该方法的精密度范围为1-4%RSD。加标于血清和尿液中的GdDTPA-BMA的回收率高于95%，RSD等于或小于4%。血清样品在-70℃储存时至少稳定5个月，尿液样品在-20℃储存时至少稳定6个月。
