摘要
设计并制作了在柱电化学(EC)检测池,用于在同一根毛细管中进行中心切割二维毛细管电泳(2DCE)在线纯化分离检测尿样中的6种β-阻断剂。尿样先在15mmol/L NaAc缓冲液中进行毛细管区带电泳(CZE)分离,带正电荷的β-阻断剂与中性和带负电荷的干扰物质分成不同区带,然后在检测端施加13.8kPa压力将干扰成分从毛细管入口端排出,同时将目标组分驱送到毛细管入口端,最后在90mmol/L NaAc-30mmol/L SDS缓冲液中进行胶束电动毛细管色谱(MEKC)分离。场放大样品堆积(FASS)/胶束推扫在柱双重富集技术不仅有效抵消压力驱送过程中产生的区带扩散,还可进一步压缩样品区带,提高检测灵敏度。本方法成功用于服药后鼠尿样品中6种β-阻断剂的分离测定,经第一维CZE分离排除干扰后,在未涂层毛细管柱(60cm×50μmi.d.)、90mmol/L NaAc/HAc-30mmol/L SDS运行缓冲液、检测电位0.8V、运行电压10kV条件下,对6种β-阻断剂进行在线富集分离,峰高、峰面积和迁移时间的相对标准偏差(RSD)分别为2.0%～4.1%,1.4%～3.7%和0.9%～2.7%(n=6)。本研究为毛细管电泳在复杂样品在线纯化分析等方面的应用提供了新方法。
A new two dimensional capillary electrophoresis with on-column electrochemical detection method was developed for online purification and separation of six β-blockers in mouse urine sample. The urine sample was firstly purified in NaAc-HAc buffer of 15 mmol/L by capillary zone electrophoresis （CZE） separation. Then, only the objective fraction of the first dimension separation was transferred to the capillary inlet end by 13.8 kPa pressure. Finally, the purified sample was separated by micellar electrokinetic capillary chromato-graphy. On column dual concentration strategies, field amplified sample stacking and sweeping, were used to overcome the peak broadening led by Taylor dispersion. This method has been successfully applied to determine β-blockers in mouse urine sample. After the urine sample was purified by CZE separation, the six β-blockers were separated in an uncoated fused silica capillary（60 cm ×50 μm i.d.） under the following conditions： background solution of 90 mmol/L NaAc/HAc＋30 mmol/L SDS, detection potential 0.8 V, running voltage 10 kV. The relative standard deviations of peak height, peak area and migration time were 2.1%-4.3%, 1.5%-3.9% and 0.7%-1.8%（n=10）, respectively. This method may be a novel procedure for the analysis of complex samples.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第5期648-652,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.20775038)
青岛科技大学博士启动基金(No.0022246)资助项目
关键词
二维毛细管电泳
中心切割
电化学检测
Β-阻断剂
Two dimensional capillary electrophoresis
Heart cutting
Electrochemical detection
β-Blocker
