Veraart J R, van Hekezen J, Groot M C, Gooijer C, Lingeman H, Velthorst N H, Brinkman U A
Vrije Universiteit, Department of Analytical Chemistry, Amsterdam, The Netherlands.
Electrophoresis. 1998 Nov;19(16-17):2944-9. doi: 10.1002/elps.1150191625.
A fully automated dialysis solid-phase extraction (SPE) sample preparation procedure is coupled on-line to capillary electrophoresis (CE) for the first time. The system is used to determine sulfonamides in serum and urine. The dialysis unit serves to remove proteins and particulate matter. Reconcentration of the analytes is performed with a small SPE column while (in)organic salts and other interferences are removed simultaneously. Finally, the analytes are desorbed and injected, via a homemade interface, into the CE system. Limits of detection (LOD) of 0.05-0.1 and 0.05-0.3 microg/mL are obtained in urine and serum, respectively. The within-day and between-day precisions are in the range of 2-6% and 3-8%, respectively, for a concentration of five times the LOD. The dialysis SPE-CE system was used over a period of six months for the analysis of over 500 serum and urine samples without problems such as clogging of the CE capillary or SPE column.
一种全自动透析固相萃取(SPE)样品制备程序首次与毛细管电泳(CE)在线联用。该系统用于测定血清和尿液中的磺胺类药物。透析单元用于去除蛋白质和颗粒物。使用小型SPE柱对分析物进行再浓缩,同时去除(有机)无机盐和其他干扰物。最后,通过自制接口将分析物解吸并注入CE系统。在尿液和血清中分别获得了0.05 - 0.1和0.05 - 0.3μg/mL的检测限(LOD)。对于五倍LOD浓度,日内和日间精密度分别在2 - 6%和3 - 8%范围内。该透析SPE - CE系统在六个月的时间里用于分析500多个血清和尿液样品,未出现CE毛细管或SPE柱堵塞等问题。