Krogh M, Grefslie H, Rasmussen K E
Institute of Pharmacy, University of Oslo, Norway.
J Chromatogr B Biomed Sci Appl. 1997 Feb 21;689(2):357-64. doi: 10.1016/s0378-4347(96)00352-0.
This paper describes microextraction and gas chromatographic analysis of diazepam from human plasma. The method was based on immobilisation of 1.5 microliters of 1-octanol on a polyacrylate-coated fiber designed for solid-phase microextraction. The solvent-modified fibre was used to extract diazepam from the samples. The plasma sample was pre-treated to release diazepam from the protein binding. The fibre was inserted into the modified plasma sample, adjusted to pH 5.5 an internal standard was added and the mixture was carefully stirred for 4 min. The fibre with the immobilised solvent and the enriched analytes was injected into the capillary gas chromatograph. The solvent and the extracted analytes were evaporated at 300 degrees C in the split-splitless injection port of the gas chromatograph, separated on a methylsilicon capillary column and detected with a nitrogen-phosphorus detector. The method was shown to be reproducible with a detection limit of 0.10 nmol/ml in human plasma.
本文描述了从人血浆中提取地西泮并进行气相色谱分析的方法。该方法基于将1.5微升1-辛醇固定在用于固相微萃取的聚丙烯酸酯涂层纤维上。使用经溶剂改性的纤维从样品中提取地西泮。对血浆样品进行预处理以使其从蛋白质结合物中释放出地西泮。将纤维插入经改性的血浆样品中，调节至pH 5.5，加入内标物，并将混合物小心搅拌4分钟。将固定有溶剂和富集分析物的纤维注入毛细管气相色谱仪中。溶剂和萃取的分析物在气相色谱仪的分流/不分流进样口中于300℃蒸发，在甲基硅毛细管柱上分离，并用氮磷检测器检测。该方法在人血浆中的检测限为0.10纳摩尔/毫升，具有可重复性。
