气泡微萃取-气相色谱-质谱法测定尿中咖啡因  

Determination of Caffeine in Urea by Bubble-in-drop Single Drop Microextraction and Gas Chromatography-Mass Spectrometry

作　　者：宋爱英[1] 王丽红 张延霞[1] 石恩林[1] 曾俊菱 

机构地区：[1]甘肃政法学院公安技术学院,兰州730070 [2]兰州军区农业新技术试验培训基地,白银730617

出　　处：《分析化学》2017年第5期707-712,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21565005);甘肃省自然科学基金(No.1506RJZA033);兰州市科技计划(No.2016-3-36)资助项目~~

摘　　要：建立了气泡微萃取结合气相色谱/质谱技术(GC-MS)测定尿中咖啡因的方法。对影响萃取效率的实验条件进行了优化,确定了最佳萃取条件:三氯甲烷作为萃取溶剂,萃取溶剂暴露体积1μL,气泡体积1.6μL,搅拌速度300 r/min,萃取时间5 min,盐度15%(m/V),气泡与磁子间距离1 cm。在优化条件下,所建立方法在咖啡因浓度0.005~10 mg/L范围内有较好的线性关系,相关系数可达0.986,检出限为0.003 mg/L。在人尿液中添加不同浓度的咖啡因(0.050、0.500和5.000 mg/L),回收率为89.2%~107.5%,相对标准偏差小于8%(n=6)。A method for the determination of caffeine in urea was developed based on bubble- in-drop single drop microextraction （ BID- SDME） followed by gas chromatography/mass spectrometry （GC-MS）. Under the optimum conditions including chloroform as extraction solvent, an exposure volume of 1 μ L, a bubble volume of 1.6 μ L, stirring for 5 min at 300 r/ min, 15% （ m/ V） NaCl, and a distance of 1 cm between bubble and stirring bar, the detection limit of this method was as low as 0. 003 mg/L and the linear range was from 0. 005 mg/L to 10 mg/L with correlation coefficient of 0. 982. The recoveries of caffeine were from 89. 2 % to 107.5% at different spiked levels in human urine and the relative standard deviation （RSD, n = 6） was less than 8 % .

关 键 词：气泡微萃取 咖啡因 气相色谱/质谱 尿 

分 类 号：R446.12[医药卫生—诊断学] O657.63[医药卫生—临床医学]