Bogusz M J, Kala M, Maier R D
Institute of Forensic Medicine, Aachen University of Technology, Germany.
J Anal Toxicol. 1997 Jan-Feb;21(1):59-69. doi: 10.1093/jat/21.1.59.
Amphetamine (A), methamphetamine (MA), methylene dioxyamphetamine (MDA), methylenedioxyethylamphelamine (MDE), and methylenedioxymethamphetamine (MDMA), as well as eight other sympathomimetic amines (benzyl-1-phenylethylamine, ephedrine, fenfluramine, norfenfluramine, phentermine, phenylethylamine, phenylpropanolamine, and propylhexedrine), were extracted from serum or urine with ether, derivatized with phenylisothiocyanate, and subjected to high-performance liquid chromatographic (HPLC) examination in isocratic mode. Two detection arts were applied: atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) and UV-spectrometry as diode array detection (DAD) or single wavelength at 250 nm. The derivatives were well-separated and showed good chromatographic behavior. Full-scan mass spectra of drugs examined by means of APCI with collision induced dissociation (APCID) contained protonated molecular ions (M+H)+ and fragments typical for particular drugs. APCID-liquid chromatography-mass spectrometry (LC-MS) appeared very selective for differentiation of all drugs involved. The quantitation with APCID was performed using selected ion monitoring (SIM) of (M+H)+ ions and selected fragments of drugs involved and their deuterated analogues. The limits of detection ranged from 0.001 mg/L (MA, MDMA, and MDE) to 0.005 mg/L (A and MDA). In HPLC-DAD, the spectra of MDMA and MDE were practically identical with maxima of 236-240 nm. Other amphetamines showed slightly different spectra with maxima of 245-250 nm. The limits of detection in UV detection amounted to 0.01-0.03 mg/L (single wavelength detector at 250 nm) or 0.05-0.1 mg/L (DAD).
苯丙胺（A）、甲基苯丙胺（MA）、亚甲二氧基苯丙胺（MDA）、亚甲二氧基乙基苯丙胺（MDE）、亚甲二氧基甲基苯丙胺（MDMA）以及其他八种拟交感神经胺（苄基-1-苯乙胺、麻黄碱、芬氟拉明、去甲芬氟拉明、苯丁胺、苯乙胺、苯丙醇胺和丙己君）用乙醚从血清或尿液中萃取，用异硫氰酸苯酯衍生化，然后在等度模式下进行高效液相色谱（HPLC）检测。采用了两种检测方法：大气压化学电离（APCI）质谱（MS）以及作为二极管阵列检测（DAD）的紫外光谱法或250nm单波长检测。衍生物分离良好，呈现出良好的色谱行为。通过带有碰撞诱导解离的APCI（APCID）检测的药物全扫描质谱包含质子化分子离子（M+H）⁺以及特定药物特有的碎片。APCID-液相色谱-质谱联用（LC-MS）对所有相关药物的区分具有很高的选择性。使用（M+H）⁺离子以及相关药物及其氘代类似物的选定碎片的选择离子监测（SIM）进行APCID定量。检测限范围从0.001mg/L（MA、MDMA和MDE）到0.005mg/L（A和MDA）。在HPLC-DAD中，MDMA和MDE的光谱几乎相同，最大吸收波长为236 - 240nm。其他苯丙胺类药物的光谱略有不同，最大吸收波长为245 - 250nm。紫外检测的检测限为0.01 - 0.03mg/L（250nm单波长检测器）或0.05 - 0.1mg/L（DAD）。
