Lee Myeongho, Oh Se Youn, Pathak Tara Sankar, Paeng Insook Rhee, Cho Byung-Yun, Paeng Ki-Jung
Department of Chemistry, Yonsei University, Wonju 220-710, South Korea.
J Chromatogr A. 2007 Aug 10;1160(1-2):340-4. doi: 10.1016/j.chroma.2007.06.033. Epub 2007 Jun 26.
A simple and selective one-step solid-phase extraction procedure using chemically modified polymer resin (Amberlite XAD-4) with crown ether was investigated for the measurement of urinary catecholamines. After loading the urine samples (adjusted to pH 4) on the synthesized adsorbent cartridge, the column was washed with methanol followed by water and then the adsorbed catecholamines were eluted by 1.0 mL of 6.0 M acetic acid. The effectiveness of sample clean-up method was demonstrated by reversed-phase ion-pair high-performance liquid chromatography with electrochemical detection. Under optimal condition, the recoveries of epinephrine, norepinephrine, and dopamine from spiked urine sample were >86% for all catecholamines. The detection limits (n=5) for epinephrine, norepinephrine, and dopamine were 37, 52, and 46 nmol/L, respectively.
研究了一种使用经冠醚化学修饰的聚合物树脂(Amberlite XAD-4)的简单且选择性的一步固相萃取方法,用于测定尿中儿茶酚胺。将尿液样本(调节至pH 4)加载到合成吸附柱上后,先用甲醇冲洗柱子,再用水冲洗,然后用1.0 mL 6.0 M乙酸洗脱吸附的儿茶酚胺。通过反相离子对高效液相色谱-电化学检测证明了样品净化方法的有效性。在最佳条件下,加标尿样中肾上腺素、去甲肾上腺素和多巴胺的回收率均>86%。肾上腺素、去甲肾上腺素和多巴胺的检测限(n=5)分别为37、52和46 nmol/L。