Tim R C, Kautz R A, Karger B L
Barnett Institute and Department of Chemistry, Northeastern University, Boston, MA, USA.
Electrophoresis. 2000 Jan;21(1):220-6. doi: 10.1002/(SICI)1522-2683(20000101)21:1<220::AID-ELPS220>3.0.CO;2-D.
This work demonstrates the use of affinity probe capillary electrophoresis (APCE) in the quantitative analysis of drugs in biological fluids at the low pM level. The interaction of human carbonic anhydrase II (HCAII) with the glaucoma drug dorzolamide (Dz) was chosen as a model system. HCAII was labeled at its single cysteine residue using a thiol-specific fluorescein reagent. The peak area of HCAII complexed with the tight-binding drug Dz provided a direct assay of the drug concentration in solution. A charged competitive ligand added to the running buffer was employed in APCE to distinguish Dz-bound from free forms of the HCAII. Using laser-induced fluorescence (LIF), the Dz detection limit was 16.5 pM in aqueous solution and 62.5 pM in both urine and plasma. Normalized peak area reproducibility of the drug was within 3.4% RSD. Each analysis was completed within 10 min, including incubation, and consumed only 0.3 pmol of labeled protein. The APCE approach provides an effective method for trace level detection of drugs in biological matrices.
这项工作展示了亲和探针毛细管电泳(APCE)在生物流体中低皮摩尔水平药物定量分析中的应用。选择人碳酸酐酶II(HCAII)与青光眼药物多佐胺(Dz)的相互作用作为模型系统。使用硫醇特异性荧光试剂对HCAII的单个半胱氨酸残基进行标记。与紧密结合药物Dz复合的HCAII的峰面积提供了溶液中药物浓度的直接测定。在APCE中,向运行缓冲液中加入带电荷的竞争性配体,以区分与Dz结合的HCAII和游离形式的HCAII。使用激光诱导荧光(LIF),Dz在水溶液中的检测限为16.5 pM,在尿液和血浆中的检测限均为62.5 pM。药物归一化峰面积的重现性在3.4%相对标准偏差(RSD)以内。每次分析在10分钟内完成,包括孵育,且仅消耗0.3皮摩尔标记蛋白。APCE方法为生物基质中药物的痕量检测提供了一种有效方法。