Determination of nonsteroidal anti-inflammatory drugs in biological fluids by automatic on-line integration of solid-phase extraction and capillary electrophoresis

被引:0
作者
Mardones, C [1 ]
Ríos, A [1 ]
Valcárcel, M [1 ]
机构
[1] Univ Cordoba, Div Analyt Chem, E-14071 Cordoba, Spain
关键词
capillary electrophoresis; flow injection analysis; solid-phase extraction; non-steroidal anti-inflammatory drugs; biological samples;
D O I
10.1002/1522-2683(200102)22:3<484::AID-ELPS484>3.0.CO;2-X
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A new, automatic method for the clean-up, preconcentration, separation, and quantitation of nonsteroidal anti-inflammatory drugs (NSAIDs) in biological samples (human urine and serum) using solid-phase extraction coupled on-line to capillary electrophoresis is proposed. Automatic pretreatment is carried out by using a continuous flow system operating simultaneously with the capillary electrophoresis equipment, to which it is linked via a laboratory-made mechanical arm. This integrated system is controlled by an electronic interface governed via a program developed in GWBasic. Capillary electrophoresis is conducted by using a separation buffer consisting of 20 mM NaHPO4, 20 mM beta -cyclodextrin and 50 mM SDS at pH 9.0, an applied potential of 20 kV and a temperature of 20 degreesC. The analysis time is 10 min and the detection limits were between 0.88 and 1.71 mug mL(-1). Automatic clean-up and preconcentration is accomplished by using a C-18 minicolumn and 75% methanol as eluent. The limit of detection of NSAIDs can be up to 400-fold improved when using sample clean-up. The extraction efficiency for these compounds is between 71.1 and 109.7 mug mL(-1) (RSD 2.0-7.7%) for urine samples and from 77.2 to 107.1 mug mL(-1) (RSD 3.5-7.1%) for serum samples.
引用
收藏
页码:484 / 490
页数:7
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