高效液相色谱-电化学法测定人尿液中儿茶酚胺的浓度
x

请在关注微信后,向客服人员索取文件

篇名: 高效液相色谱-电化学法测定人尿液中儿茶酚胺的浓度
TITLE:
摘要: 目的:建立测定人尿液中儿茶酚胺浓度的方法。方法:尿液样品经氧化铝提取后,以3,4-二羟基苄胺为内标,采用高效液相色谱-电化学法测定,色谱柱为Shim-Pack C18,流动相为混合溶液[每500 ml混合溶液中含离子对试剂(辛烷磺酸钠)0.5 mmol、甲醇10 ml、0.06 mmol/L二正丁胺50 μl、无水乙酸钠2.0 g、柠檬酸5.5 g、乙二胺四乙酸二钠60 mg和氯化钠584.4 mg,pH=3.5],流速为0.8 ml/min,柱温为30 ℃,电化学检测器检测电压为750 mV,进样量为40 μl。结果:去甲肾上腺素和肾上腺素的尿药浓度均在3.125~100 ng/ml范围内线性关系良好(r分别为0.998 5和0.999 2),定量下限均为3.125 ng/ml;日内、日间RSD均<10%;方法回收率分别为99.2%~101.6%、98.9%~100.5%,提取回收率分别为63.8%~66.8%、60.5%~62.6%。结论:本方法特异性强、灵敏度较高、检测成本低,可用于人尿液中儿茶酚胺浓度的测定。
ABSTRACT: OBJECTIVE: To establish a method for the concentration determination of catecholamines in human urine. METHODS: After extracted by aluminum oxide, using 3, 4-dihydroxybenzylamine as internal standard, HPLC-electrochemistry was performed on the column of Shim-Pack C18 with mixed solution [every 500 ml mixed solution containing ion-pairing reagents (octane sulfonate) 0.5 mmol, methanol 10 ml, 0.06 mmol/L Di-n-butylamine 50 μl, sodium acetate anhydrous 2.0 g, citric acid 5.5 g, EDTA-Na2 60 mg and sodium chloride 584.4 mg, pH=3.5] at a flow rate of 0.8 ml/min, column temperature was 30 ℃, detection voltage was 750 mV, and injection volume was 40 μl. RESULTS: The linear ranges were 3.125-100 ng/ml for both norepinephrine (r=0.998 5) and epinephrine (r=0.999 2), lower limits of quantitation were 3.125 ng/ml; RSDs of within days and daytime were lower than 10%, method recoveries were 99.2%-101.6% and 98.9%-100.5%, extraction recoveries were 63.8%-66.8% and 60.5%-62.6%. CONCLUSIONS: The method shows strong specificity, high sensitivity and low detection cost, and can be used for the concentration determination of catecholamines in human urine.
期刊: 2016年第27卷第26期
作者: 陈静,丘宏强
AUTHORS: CHEN Jing,QIU Hongqiang
关键字: 儿茶酚胺;去甲肾上腺素;肾上腺素;高效液相色谱法;电化学检测器;尿液
KEYWORDS: Catecholamines; Norepinephrine; Epinephrine; HPLC; Electrochemical detector; Urine
阅读数: 280 次
本月下载数: 4 次

* 注:未经本站明确许可,任何网站不得非法盗链资源下载连接及抄袭本站原创内容资源!在此感谢您的支持与合作!