Yang GuiDi, Xu JinHua, Zheng JinPing, Xu XueQin, Wang Wei, Xu LiangJun, Chen GuoNan, Fu FengFu
Key Laboratory of Analysis and Detection Technology for Food Safety of Ministry of Education and Department of Chemistry, Fuzhou University, Fuzhou, Fujian 350108, China.
Talanta. 2009 Apr 30;78(2):471-6. doi: 10.1016/j.talanta.2008.11.040. Epub 2008 Dec 3.
An improved sheath-flow interface used to couple capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICP-MS) and a microwave-assisted extraction used to extract each arsenic species in seafood were developed in this work. The improved sheath-flow interface completely avoids laminar flow in CE capillary caused by the suction from ICP-MS, makes electric supply more stable in CE, and transports analyte solution to ICP-MS easily and more efficiently. CE-ICP-MS coupled with our interface have two quantitative analysis modes: continuous sample-introduction mode and collective sample-introduction mode. The collective sample-introduction technique greatly reduced the dead volume of interface to approximately zero, obviously avoided the excessive dilution of analyte, and eventually led to a much lower detection limit and a much better electrophoretic resolution. This was demonstrated by the better symmetry and narrow peak widths (10-12s) and much lower detection limits (0.030-0.042 microg/L) of four species of arsenic determined with collective sample-introduction mode. With the help of this improved sheath-flow interface and the microwave-assisted extraction, we have successfully separated and determined four arsenic species, As(III), As(V), monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) in dried Mya arenaria Linnaeus and Shrimp samples using CE-ICP-MS within 10 min with a relative standard deviation of 2-4% (peak areas, n=6) and a recovery of 96-105%.
本研究开发了一种改进的鞘流接口,用于将毛细管电泳(CE)与电感耦合等离子体质谱(ICP-MS)联用,以及一种微波辅助萃取方法,用于萃取海鲜中的各种砷形态。改进后的鞘流接口完全避免了因ICP-MS抽吸导致的CE毛细管中的层流现象,使CE中的供电更加稳定,并能更轻松、高效地将分析物溶液输送至ICP-MS。采用我们的接口联用的CE-ICP-MS有两种定量分析模式:连续进样模式和集中进样模式。集中进样技术将接口的死体积大幅降低至接近零,明显避免了分析物的过度稀释,最终实现了更低的检测限和更好的电泳分辨率。这通过集中进样模式测定的四种砷形态具有更好的对称性和更窄的峰宽(10 - 12秒)以及更低的检测限(0.030 - 0.042微克/升)得到了证明。借助这种改进的鞘流接口和微波辅助萃取,我们成功地使用CE-ICP-MS在10分钟内分离并测定了沙海螂干品和虾类样品中的四种砷形态,即As(III)、As(V)、一甲基砷酸(MMA)和二甲基砷酸(DMA),相对标准偏差为2 - 4%(峰面积,n = 6),回收率为96 - 105%。