Soetebeer U B, Schierenberg M O, Schulz H, Grünefeld G, Andresen P, Blaschke G
Institute of Pharmaceutical Chemistry, University of Münster, Germany.
J Chromatogr B Biomed Sci Appl. 2000 Aug 18;745(2):271-8. doi: 10.1016/s0378-4347(00)00280-2.
Capillary electrophoresis (CE) with UV laser-induced native fluorescence detection was developed as a sensitive and selective assay for the direct determination of tramadol in human urine without extraction or preconcentration. The main problem in CE is the small inner diameter of the capillary which causes a low sensitivity with instruments equipped with a UV detector. Laser-induced native fluorescence with a frequency doubled argon ion laser at an excitation wavelength of 257 nm was used for the direct assay of tramadol in urine to enhance the limit of detection about 1,000-fold compared to UV absorption detection. The detection system consists of an imaging spectrograph and an intensified CCD camera, which views an illuminated 1.5 mm section of the capillary. This set-up is able to record the whole emission spectra of the analytes to achieve additionally wavelength-resolved electropherograms. In the concentration range of 20 ng/ml-5 microg/ml in human urine coefficients of correlation were better than 0.998. Within-day variation determined on four different concentrations showed accuracies ranging from 90.2 to 108.4%. The relative standard deviation (RSD) was determined to be less than 10%. Day-to-day variation presented accuracies ranging from 90.9 to 103.1% with an RSD less than 8%.
采用紫外激光诱导天然荧光检测的毛细管电泳（CE）技术被开发为一种灵敏且选择性强的分析方法，用于直接测定人尿液中的曲马多，无需萃取或预浓缩。毛细管电泳的主要问题在于毛细管内径较小，这使得配备紫外检测器的仪器灵敏度较低。使用波长为257nm的倍频氩离子激光诱导天然荧光，用于直接检测尿液中的曲马多，与紫外吸收检测相比，检测限提高了约1000倍。检测系统由成像光谱仪和增强型电荷耦合器件（CCD）相机组成，该相机可观察毛细管1.5mm的光照部分。这种设置能够记录分析物的整个发射光谱，以获得额外的波长分辨电泳图。在人尿液中20ng/ml - 5μg/ml的浓度范围内，相关系数优于0.998。在四种不同浓度下测定的日内变化显示，准确度范围为90.2%至108.4%。相对标准偏差（RSD）测定值小于10%。日间变化的准确度范围为90.9%至103.1%，RSD小于8%。
