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50μl、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40μl。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。
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-Na260 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% and60.5%-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.
出处
《中国药房》
CAS
北大核心
2016年第26期3627-3629,共3页
China Pharmacy
