气泡微萃取-气相色谱-质谱法测定尿中咖啡因

引用本文: 宋爱英, 王丽红, 张延霞, 石恩林, 曾俊菱. 气泡微萃取-气相色谱-质谱法测定尿中咖啡因[J]. 分析化学, 2017, 45(5): 707-712. doi: 10.11895/j.issn.0253-3820.160862 shu

Citation: SONG Ai-Ying, WANG Li-Hong, ZHANG Yan-Xia, SHI En-Lin, ZENG Jun-Ling. Determination of Caffeine in Urea by Bubble-in-drop Single Drop Microextraction and Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(5): 707-712. doi: 10.11895/j.issn.0253-3820.160862 shu

气泡微萃取-气相色谱-质谱法测定尿中咖啡因

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
基金项目:
本文系国家自然科学基金（No. 21565005）、甘肃省自然科学基金（No. 1506RJZA033）和兰州市科技计划（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1 μL，气泡体积1.6 μL，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）。

关键词:

English

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

1.
School of Public Security & Technology, Gansu Institute of Political Science and Law, Lanzhou 730070, China;
2.
Practice and Training Bases for New Agricultural Technology, Lanzhou Military Area Command of Chinese People's Liberation Army, Baiyin 730617, China
Received Date: 24 November 2016
Revised Date: 15 March 2017
Fund Project:
This work was supported by the National Natural Science Foundation of China (No. 21565005), the Natural Science Foundation of Gansu Province, China (No. 1506RJZA033) and the Project on Science and Technology of Lanzhou City (No. 2016-3-36)

Abstract: 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 μL, a bubble volume of 1.6 μL, 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%.

Key words:

Bubble-in-drop single drop microextraction
/ Caffeine
/ Gas chromatography-mass spectrometry
/ Urea

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沈阳化工大学材料科学与工程学院沈阳 110142

气泡微萃取-气相色谱-质谱法测定尿中咖啡因

English

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

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

气泡微萃取-气相色谱-质谱法测定尿中咖啡因

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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