Gu Congying, Lin Li, Li Bin, Chen Xiaodong, Ren Jicun, Jia Jinping, Wu Dan, Fang Nenghu
College of Environmental Science and Engineering, Shanghai Jiaotong University, Shanghai, P. R. China.
Electrophoresis. 2008 Sep;29(18):3887-95. doi: 10.1002/elps.200700944.
As a new wave of technology, polymethacrylate-based monolithic column was prepared and its application in the separation of three kinds of microcystins (MCs) in pressurized capillary electrochromatography with ultraviolet detection was studied. The key factors affecting the separation performance, such as monolithic column, pressure of the pump, component and concentration of mobile phase and the voltage, were investigated and optimized in detail. A baseline separation could be achieved in less than 6 min using a 5 mM borate buffer with a pH of 9.6 and 10% acetonitrile as the mobile phases in isocratic elution, under a voltage of +13 kV and a supplementary pressure of 7.5 MPa. The calibration curves were linear with correlation coefficient r>0.998 over a range of 0.10-25.00 mg/L. The LODs for the three MCs were in the range of 0.03-0.09 mg/L. This method was successfully applied to separate MCs from other compounds in spiked tap water after solid-phase extraction. The lower LODs for MC-LR, MC-YR and MC-RR were obtained to be 0.10, 0.13, 0.16 microg/L, respectively. These results make it clear that this proposed system is accurate and robust enough to be used as a fast separation tool for routine monitoring of MCs in real water samples.
作为一种新技术浪潮，制备了基于聚甲基丙烯酸酯的整体柱，并研究了其在加压毛细管电色谱-紫外检测中用于分离三种微囊藻毒素（MCs）的应用。详细研究并优化了影响分离性能的关键因素，如整体柱、泵压、流动相的组成和浓度以及电压。在等度洗脱中，使用pH为9.6的5 mM硼酸盐缓冲液和10%乙腈作为流动相，在+13 kV电压和7.5 MPa补充压力下，不到6分钟即可实现基线分离。校准曲线在0.10 - 25.00 mg/L范围内呈线性，相关系数r>0.998。三种MCs的检测限在0.03 - 0.09 mg/L范围内。该方法成功应用于固相萃取后从加标自来水中分离MCs与其他化合物。MC-LR、MC-YR和MC-RR的较低检测限分别为0.10、0.13、0.16 μg/L。这些结果表明，该系统准确且稳健，足以作为实际水样中MCs常规监测的快速分离工具。
