de Zeeuw R A, Wijsbeek J, Franke J P
Department of Analytical Chemistry and Toxicology, University Centre for Pharmacy, Groningen, The Netherlands.
J Anal Toxicol. 2000 Mar;24(2):97-101. doi: 10.1093/jat/24.2.97.
Broad-spectrum drug screening requires that all relevant substances be isolated, detected, and identified, regardless of their structure and/or polarity. To this end, systematic solid-phase extraction (SPE) approaches for drug isolation from biological fluids are required. Because speed and cost effectiveness are key issues in analytical toxicology, we have evaluated a disc-format extraction device for this purpose and compared the latter with an existing packed-bed column-format method. The discs were SPEC.PLUS.C18AR/MP3 cartridges with 10-mL solvent reservoirs, providing hydrophobic and cation exchange interactions. Blank human urine was spiked at 2 microg/mL with a selection of acidic, neutral, and basic drugs representing a variety of relevant drug classes. Urine specimens (2 mL) were diluted with 2 mL 0.1 M phosphate buffer (pH 5.0) and then applied to the preconditioned disc. Washing was done with 1 mL water. Acidic and neutral drugs were eluted with 1 mL ethyl acetate/acetone (1:1), and basic drugs were eluted with 1 mL ammoniated ethyl acetate. The eluates were collected separately, evaporated down to about 0.1 mL, and analyzed by gas chromatography-flame-ionization detection to check cleanliness, recoveries, and reproducibilities. The discs showed good extraction properties for all drugs and were easy to handle. Recoveries were 75-100% with coefficients of variation of around 5%. The resulting eluates showed only a few matrix interferences. As compared to our standard SPE method with packed-bed columns, the disc procedure allowed reductions in elution volumes and total processing time of approximately 60-65%.
广谱药物筛选要求分离、检测和鉴定所有相关物质，无论其结构和/或极性如何。为此，需要采用系统的固相萃取（SPE）方法从生物流体中分离药物。由于速度和成本效益是分析毒理学中的关键问题，我们为此评估了一种圆盘式萃取装置，并将其与现有的填充床柱式方法进行了比较。这些圆盘是带有10 mL溶剂储液器的SPEC.PLUS.C18AR/MP3柱芯，可提供疏水和阳离子交换相互作用。向空白人尿中加入2 μg/mL的一系列酸性、中性和碱性药物，这些药物代表了各种相关的药物类别。将尿液标本（2 mL）用2 mL 0.1 M磷酸盐缓冲液（pH 5.0）稀释，然后加至预处理过的圆盘上。用1 mL水进行洗涤。酸性和中性药物用1 mL乙酸乙酯/丙酮（1:1）洗脱，碱性药物用1 mL氨化乙酸乙酯洗脱。分别收集洗脱液，蒸发至约0.1 mL，然后通过气相色谱-火焰离子化检测进行分析，以检查清洁度、回收率和重现性。这些圆盘对所有药物均显示出良好的萃取性能，且易于操作。回收率为75 - 100%，变异系数约为5%。所得洗脱液仅显示出少量的基质干扰。与我们采用填充床柱的标准SPE方法相比，圆盘法可使洗脱体积和总处理时间减少约60 - 65%。
