Slawson Matthew H, Taccogno James L, Foltz Rodger L, Moody David E
Department of Pharmacology and Toxicology, University of Utah Health Sciences Center, Salt Lake City 84112, USA.
J Anal Toxicol. 2002 Oct;26(7):430-7. doi: 10.1093/jat/26.7.430.
This report describes a sensitive and specific high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry method for the detection of subnanogram concentrations of selegiline and its three principle metabolites, N-desmethylselegiline, methamphetamine, and amphetamine, in human plasma. The assay has a dynamic range of 0.1-20 ng/mL for selegiline and N-desmethylselegiline (norselegiline) and 0.2-20 ng/mL for methamphetamine and amphetamine. The inter- and intra-assay precision and accuracy varied by less than 11% for all analytes at 0.3, 2.5, and 15 ng/mL and less than 16% at the lower limit of quantitation (0.1 ng/mL for selegiline and norselegiline; and 0.2 ng/mL for methamphetamine and amphetamine). Selegiline and its metabolites showed no significant loss in quantitative accuracy after three freeze/thaw cycles or after up to 6 h at room temperature prior to extraction. Extracted plasma samples retained quantitative accuracy after storage for at least 7 days at -20 degrees C or up to 70 h at room temperature. Methanolic stock solutions were stable for at least 6 h when kept at room temperature or at least 90 days when kept at -20 degrees C.
本报告描述了一种灵敏且特异的高效液相色谱 - 大气压化学电离 - 串联质谱法，用于检测人血浆中亚纳克级浓度的司来吉兰及其三种主要代谢物，即N - 去甲基司来吉兰、甲基苯丙胺和苯丙胺。该检测方法对司来吉兰和N - 去甲基司来吉兰（去甲司来吉兰）的动态范围为0.1 - 20 ng/mL，对甲基苯丙胺和苯丙胺的动态范围为0.2 - 20 ng/mL。在0.3、2.5和15 ng/mL浓度下，所有分析物的批间和批内精密度及准确度变化均小于11%，在定量下限（司来吉兰和去甲司来吉兰为0.1 ng/mL；甲基苯丙胺和苯丙胺为0.2 ng/mL）时变化小于16%。经过三次冻融循环或在提取前于室温放置长达6小时后，司来吉兰及其代谢物的定量准确度无显著损失。提取后的血浆样品在 -20℃下储存至少7天或在室温下储存长达70小时后仍保持定量准确度。甲醇储备溶液在室温下保存至少6小时稳定，在 -20℃下保存至少90天稳定。
