Pelander Anna, Backström Daniel, Ojanperä Ilkka
Department of Forensic Medicine, P.O. Box 40, University of Helsinki, FIN-00014 Helsinki, Finland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Oct 1;857(2):337-40. doi: 10.1016/j.jchromb.2007.07.031. Epub 2007 Aug 2.
An overpressured layer chromatography (OPLC) method was evaluated for broad-scale screening of basic drugs in 5g autopsy liver samples using two parallel OPLC systems. Sample preparation included enzymatic digestion with trypsin and liquid-liquid extraction with butyl chloride. Chromatographic separation was performed as dual-plate analysis, with mobile phases composed of trichloroethylene-methylethylketone-n-butanol-acetic acid-water (17:8:25:6:4, v/v) (OPLC1), and butyl acetate-ethanol (96.1%)-tripropylamine-water (85:9.25:5:0.75, v/v). Identification was based on automated comparison of corrected R(f) values (hR(f)c) and in situ UV spectra with library values by dedicated software. The identification limit was determined for 25 basic drugs in liver ranging from 0.5 to 10mg/kg. The OPLC method proved to be well suited for routine screening analysis of basic drugs in post-mortem samples of varying quality, combining the benefit from moderately high separation power with the ease of disposable plates.
使用两个平行的过压薄层色谱（OPLC）系统，对5g尸检肝脏样本中的碱性药物进行大规模筛查，对OPLC方法进行了评估。样品制备包括用胰蛋白酶进行酶消化和用丁基氯进行液-液萃取。色谱分离采用双板分析，流动相由三氯乙烯-甲乙酮-正丁醇-乙酸-水（17:8:25:6:4，v/v）（OPLC1）和乙酸丁酯-乙醇（96.1%）-三丙胺-水（85:9.25:5:0.75，v/v）组成。通过专用软件将校正后的比移值（hR(f)c）和原位紫外光谱与库值进行自动比较来进行鉴定。确定了肝脏中25种碱性药物的鉴定限，范围为0.5至10mg/kg。OPLC方法被证明非常适合对不同质量的死后样本中的碱性药物进行常规筛查分析，它结合了适度高分离能力的优点和一次性板的便利性。
