Swynnerton N F, McGovern E P, Niño J A, Mangold D J
Int J Radiat Oncol Biol Phys. 1984 Sep;10(9):1521-4. doi: 10.1016/0360-3016(84)90494-2.
An HPLC assay is presented for the detection and quantitation of the radioprotective drug S-2-(3-aminopropylamino)ethyl phosphorothioate (WR-2721, ethiofos) present in plasma. Improved selectivity and a 40-fold increase in sensitivity have been demonstrated over the method previously reported by this laboratory. Using precolumn derivatization with fluorescamine and S-3-(4-aminobutylamino)propyl phosphorothioate (WR-80855, a homolog of WR-2721) as the internal standard, drug levels of 0.05 to 1000 micrograms/mL were determined with excellent precision (CV less than or equal to 5% over the concentration range). An isocratic mobile phase of acetonitrile/ethanol/water (16:7:77) modified with 0.01 M tetrabutylammonium phosphate eluted the drug and the internal standard from the C-18 reverse-phase column in 23 minutes and 26 minutes, respectively. Detector response was linear over the entire range. The assay uses 150 microL of plasma and requires a total chromatography time of about 50 minutes. The method was found suitable for pharmacokinetic studies in a preliminary experiment with a beagle dog in which no interferences due to plasma constituents or drug metabolites were observed.
本文介绍了一种用于检测和定量血浆中放射防护药物S-2-(3-氨丙基氨基)乙基硫代磷酸酯（WR-2721，乙磺磷）的高效液相色谱法。与本实验室先前报道的方法相比，该方法具有更高的选择性，灵敏度提高了40倍。采用荧光胺柱前衍生化，以S-3-(4-氨丁基氨基)丙基硫代磷酸酯（WR-80855，WR-2721的同系物）作为内标，可精确测定0.05至1000微克/毫升的药物浓度（在该浓度范围内变异系数小于或等于5%）。用0.01 M磷酸四丁铵改性的乙腈/乙醇/水（16:7:77）等度流动相分别在23分钟和26分钟内将药物和内标从C-18反相柱上洗脱下来。在整个范围内，检测器响应呈线性。该检测方法使用150微升血浆，总色谱分析时间约为50分钟。在对一只比格犬进行的初步实验中，该方法被证明适用于药代动力学研究，未观察到血浆成分或药物代谢物的干扰。
