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目的:采用弱阳离子固相萃取小柱(WCX-SPE)优化人血浆儿茶酚胺检测实验条件,以减少血浆用量,提高实验稳定性,建立操作简单、可靠的人血浆儿茶酚胺浓度检测方法。方法:采用waters WCX固相萃取小柱提取血浆中儿茶酚胺,采用高效液相色谱-电化学检测法测定儿茶酚胺,并对其线性范围、方法回收率、提取回收率、日间日内精密度及稳定性进行考察。结果:去甲肾上腺素(NE)在50~2 000 pg·ml-1(n=6,r=0.998 5),肾上腺素(E)在50~2 000 pg·ml-1(n=6,r=0.999 3)浓度范围内线性关系良好,最低检测限分别为25,50 pg·ml-1(S/N≥3),NE、E样品的平均提取回收率分别为89.6%、91.5%,平均方法回收率分别为100.6%,99.4%,平均日间RSD分别为5.1%,4.3%,平均日内RSD分别为3.9%,3.6%。结论:采用WCX固相萃取小柱提取血浆中儿茶酚胺灵敏度高,操作简便,结果准确可靠,适合于临床诊疗需要。
OBJECTIVE: To optimize the method for the determination of catecholamines in human plasma by using WCX-SPE, to reduce the amount of plasma and improve the stability of the experiment, and to establish a simple and reliable method for the determination of catecholamine in human plasma. Methods: The plasma catecholamines were extracted by waters WCX cartridge and the catecholamines were determined by high performance liquid chromatography-electrochemical detection. The linear range, recovery, extraction recovery, intra-day precision and stability To inspect. (N = 6, r = 0.998 5), epinephrine (E) was 50-2 000 pg · ml-1 (n = 6, r = 0.999 3). The detection limits were 25,50 pg · ml-1 (S / N≥3) respectively. The average extraction recoveries of NE and E samples were 89.6% and 91.5%, respectively. The average recovery rates were 100.6% and 99.4%, respectively. The average daytime RSD was 5.1% and 4.3% respectively. The average daily RSD was 3.9% and 3.6% respectively. Conclusion: The WCX solid phase extraction cartridge for plasma catecholamine high sensitivity, easy to operate, the results are accurate and reliable, suitable for clinical diagnosis and treatment needs.