Frost M, Köhler H, Blaschke G
Institute of Legal Medicine, Westfälische Wilhelms-Universität, Münster, Germany.
J Chromatogr B Biomed Sci Appl. 1997 Jun 6;693(2):313-9. doi: 10.1016/s0378-4347(97)00093-5.
Capillary electrophoresis (CE) with HeCd laser-induced fluorescence (LIF) detection and its application in forensic toxicology is demonstrated by the determination of D-lysergic acid diethylamide (LSD) in blood. Following precipitation of proteins, washing of the evaporated supernatant and extraction, the residue was reconstituted in methanol and injected electrokinetically (10 s, 10 kV). The total analysis time for quantification of LSD was 8 min using a citrate-methanol buffer, pH 4.0. With this buffer system it is possible to separate LSD, nor-LSD, iso-LSD and iso-nor-LSD. Using a specific sample preparation, electrokinetic injection, extended light path (bubble cell) capillaries and especially LIF detection (lambda(ex) 325 nm, lambda(em) 435 nm), a limit of detection of 0.1-0.2 ng LSD per ml blood could be obtained. The limit of quantitation was about 0.4-0.5 ng/ml. The quantitative evaluation for LSD was carried out using methylergometrine as internal standard. The precision expressed as coefficient of variation (C.V.) and accuracy of the method were <20% and 86-110%, respectively. The application of the method to human blood samples from two forensic cases and a comparison with radioimmunoassay demonstrated that the results were consistent.
通过测定血液中的D-麦角酸二乙酰胺(LSD),展示了采用氦镉激光诱导荧光(LIF)检测的毛细管电泳(CE)及其在法医毒理学中的应用。蛋白质沉淀、洗涤蒸发后的上清液并进行萃取后,将残渣用甲醇复溶并进行电动进样(10秒,10千伏)。使用pH 4.0的柠檬酸盐-甲醇缓冲液,定量LSD的总分析时间为8分钟。使用该缓冲系统,可以分离LSD、去甲LSD、异LSD和异去甲LSD。采用特定的样品制备、电动进样、长光程(气泡池)毛细管,特别是LIF检测(激发波长325纳米,发射波长435纳米),可获得每毫升血液中0.1 - 0.2纳克LSD的检测限。定量限约为0.4 - 0.5纳克/毫升。以甲基麦角新碱作为内标对LSD进行定量评估。以变异系数(C.V.)表示的精密度和该方法的准确度分别<20%和86 - 110%。将该方法应用于两起法医案件的人体血液样本,并与放射免疫分析进行比较,结果表明两者一致。