Martins Liliane, Yegles Michel, Chung Heesun, Wennig Robert
National Laboratory of Health, Toxicology Division, University of Luxembourg, CRP-Santé, 162A, Avenue de la Faïencerie, Luxembourg L-1511, Luxembourg.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Oct 15;825(1):57-62. doi: 10.1016/j.jchromb.2004.12.037. Epub 2005 Jan 27.
Enantioselective quantification of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA) enantiomers in hair using gas chromatography-mass spectrometry (GC-MS) is described. Hair specimens were digested with 1M sodium hydroxide at 100 degrees C for 30 min and extracted by a solid phase procedure using Cleanscreen ZSDAU020. Extracted analytes were derivatised with (S)-heptafluorobutyrylprolyl chloride and the resulting diastereoisomers were quantified by GC-MS operating in the negative chemical ionization mode. Extraction yields were between 73.0 and 97.9%. Limits of detection varied in the range of 2.1-45.9 pg/mg hair, whereas the lowest limits of quantification varied between 4.3 and 91.8 pg/mg hair. Intra- and inter-assay precision and respective accuracy were acceptable. The enantiomeric ratios (R versus S) of AM, MA, MDA, MDMA and MDEA were determined in hair from suspected amphetamine abusers. Only MA and AM enantiomers were detectable in this collective and the quantification data showed in most cases higher concentrations of (R)-MA and (R)-AM than those of the corresponding (S)-enantiomers.
描述了使用气相色谱-质谱联用仪(GC-MS)对毛发中的苯丙胺(AM)、甲基苯丙胺(MA)、3,4-亚甲基二氧基苯丙胺(MDA)、3,4-亚甲基二氧基甲基苯丙胺(MDMA)和3,4-亚甲基二氧基乙基苯丙胺(MDEA)对映体进行对映选择性定量分析的方法。毛发样本在100℃下用1M氢氧化钠消化30分钟,然后使用Cleanscreen ZSDAU020通过固相程序进行萃取。萃取的分析物用(S)-七氟丁酰基丙酰氯进行衍生化,所得非对映异构体通过在负化学电离模式下运行的GC-MS进行定量分析。萃取率在73.0%至97.9%之间。检测限在2.1-45.9 pg/mg毛发范围内变化,而最低定量限在4.3-91.8 pg/mg毛发之间变化。批内和批间精密度以及各自的准确度均可接受。在疑似苯丙胺滥用者的毛发中测定了AM、MA、MDA、MDMA和MDEA的对映体比例(R对S)。在该群体中仅可检测到MA和AM对映体,定量数据显示在大多数情况下,(R)-MA和(R)-AM的浓度高于相应的(S)-对映体。