顶空液相微萃取-胶束电动毛细管色谱分析药品中酯类防腐剂  

Determination of p-Hydroxybenzoate Preservatives in Medicine by Headspace Liquid Phase Microextraction and Micellar Electrokinetic Capillary Chromatography

作　　者：高勇[1] 何友昭[1] 谢海洋[1] 凌妲思[1] 

机构地区：[1]中国科学技术大学化学系,合肥230026

出　　处：《分析化学》2010年第11期1625-1628,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20675075)资助项目

摘　　要：建立了在同一根毛细管上实施萃取剂定容、微液滴悬挂、富集液注入和胶束电动毛细管色谱分析的一体化顶空液相微萃取#胶束电动毛细管色谱联用技术,并将其用于药品中对羟基苯甲酸酯类防腐剂的分析。将二甲亚砜-甲苯(1∶4,V/V)混合萃取剂(避免接触皮肤)用压力充满容积约1μL的分离毛细管,再从毛细管末端用压力将含150mmol/L十二烷基硫酸钠的20mmol/L硼砂缓冲液(pH9.3)充满毛细管,同时推出萃取剂,使溶剂微液滴悬挂于毛细管进样端;在加入8mL样品溶液(含0.3g/mL NaCl)的14mL样品瓶中,以90℃顶空萃取30min;高差10cm进样20s后,进行胶束电动毛细管色谱分析。对羟基苯甲酸甲、乙和丙酯的富集倍数为25～86,检出限为0.01～0.05mg/L,回收率为92.2%～107%。此联用技术可有效富集中性分析物,消除样品基体干扰,适用于复杂基体样品内中性分析物的毛细管电泳分析。An integrative coupling technique of headspace liquid phase microextraction （ HS-LPME） and micellar electrokinetic capillary chromatography （ MEKC ） was proposed and applied to analyze p-hydroxybenzoate preservatives in medicine. The analytical technique was performed with one separation capillary to fix the acceptor volume,hold the microextraction droplet,inject the concentrated analytes and separate the analytes by MEKC. First,a mixed solvent of 1∶4（ V/V） dimethylsulfoxide-toluene （ avoid contact with skin） was injected into the whole separation capillary with the volume about 1 μL from its outlet by pressure,then a running buffer solution of 20 mmol/L sodium tetraborate （ pH 9. 3） containing 150 mmol/L sodium dodecylsulfate was injected at 35 kPa for 25 s in the same direction and a 1 μL microextraction droplet was formed at the inlet of the capillary. The HS-LPME was carried out in a 14-mL sample viel containing 8 mL sample solution and 0. 3 g/mL NaCl at 90 ℃ for 30 min. At last,the concentrated analytes were injected at 10 cm height difference for 20 s and separated by MEKC. The enrichment factors of methyl-,ethyland propyl-parabens ranged from 25 to 86,the limits of detection were from 0. 01 to 0. 05 mg/L,and the recoveries were in the range of 92. 2% 107. 0% . The integrative coupling technique was able to concentrate analytes and eliminate the matrix interference effectively,and was suitable for the determination of neutral analytes in complex samples by CE

关 键 词：顶空液相微萃取 胶束电动毛细管色谱 对羟基苯甲酸酯 防腐剂 

分 类 号：TQ460.7[化学工程—制药化工]