Webb K S, Baker P B, Cassells N P, Francis J M, Johnston D E, Lancaster S L, Minty P S, Reed G D, White S A
Laboratory of the Government Chemist, Teddington, Middlesex, England.
J Forensic Sci. 1996 Nov;41(6):938-46.
A forensic procedure for the screening and confirmation of the presence of lysergide (lysergic acid diethylamide, LSD) in urine is described together with the evaluation of a novel enzyme immunoassay (EIA) and immunoaffinity extraction procedure. Following initial screening using either an established radioimmunoassay (RIA) or a novel EIA procedure, a quantitative estimate is established using a conventional high performance liquid chromatography-fluorescence (HPLC) technique following solid phase extraction. Final confirmation and quantitation, without derivatization, is established using HPLC in combination with electrospray ionization (ESI) mass spectrometry using methysergide as an internal standard. The detection limit of LSD in urine is 0.5 ng/mL. A blind trial confirmed the validity of the results. The choice of internal standard is discussed. Consideration is given to the photosensitivity of LSD solutions. A study of potential interferants in the HPLC-MS confirmation of LSD is presented and shows that for the wide range of compounds studied, there are none that would interfere with this confirmation technique. A comparison is shown between solid phase and immunoaffinity extraction/clean up procedures, and between RIA and EIA screening procedures.
本文描述了一种用于筛查和确认尿液中麦角酰二乙胺(LSD)存在的法医程序,以及对一种新型酶免疫分析(EIA)和免疫亲和萃取程序的评估。在使用既定的放射免疫分析(RIA)或新型EIA程序进行初步筛查后,采用固相萃取后的传统高效液相色谱 - 荧光(HPLC)技术进行定量估计。使用HPLC结合电喷雾电离(ESI)质谱法并以甲基麦角新碱作为内标,在不进行衍生化的情况下进行最终确认和定量。尿液中LSD的检测限为0.5 ng/mL。一项盲法试验证实了结果的有效性。讨论了内标的选择。考虑了LSD溶液的光敏性。介绍了在HPLC-MS确认LSD时对潜在干扰物的研究,结果表明,在所研究的广泛化合物范围内,没有会干扰该确认技术的物质。展示了固相萃取与免疫亲和萃取/净化程序之间以及RIA和EIA筛查程序之间的比较。