Marchei Emilia, Pellegrini Manuela, Pacifici Roberta, Zuccaro Piergiorgio, Pichini Simona
Drug Control and Evaluation Department, Istituto Superiore di Sanitá, V.le Regina Elena 299, 00161 Rome, Italy.
J Pharm Biomed Anal. 2006 Aug 28;41(5):1633-41. doi: 10.1016/j.jpba.2006.02.043. Epub 2006 Mar 31.
A simple method for the determination of ephedrine alkaloids: ephedrine (EF), pseudoephedrine (PE), norpseudoephedrine (NPE), norephedrine (NE) and methylpseudoephedrine (MPE) in dietary supplements by gas chromatography-mass spectrometry is described. After the addition of 3,4-methylenedioxypropylamphetamine as internal standard, a liquid-liquid extraction procedure in alkaline conditions with chloroform/isopropanol (9:1, v/v) was applied to the samples prior to analysis. Chromatography was performed on a fused capillary column and analytes, derivatized with pentafluoropropionic anhydride, were determined in the selected-ion-monitoring (SIM) mode. The method was validated in the range 0.3-10 microg/mg for EP, 0.06-2.5 microg/mg for PE and NPE and 0.04-1 microg/mg NE and MPE. Mean recovery ranged between 65.7 and 81.3% for the different analytes in dietary supplements. The quantification limits were 0.3 microg/mg for EP, 0.06 microg/mg for PE, 0.04 microg/mg for NPE, NE and MPE. The method was applied to analysis of various dietary supplements containing Ma-huang (Ephedra Sinica) and Sida Cordifolia plant extracts promoted for aiding weight control and boosting sports performance and energy.
描述了一种通过气相色谱 - 质谱法测定膳食补充剂中麻黄碱类生物碱的简单方法：麻黄碱（EF）、伪麻黄碱（PE）、去甲伪麻黄碱（NPE）、去甲麻黄碱（NE）和甲基伪麻黄碱（MPE）。加入3,4 - 亚甲基二氧丙基苯丙胺作为内标后，在分析前对样品采用碱性条件下用氯仿/异丙醇（9:1，v/v）的液 - 液萃取程序。在熔融毛细管柱上进行色谱分析，用五氟丙酸酐衍生化的分析物在选择离子监测（SIM）模式下测定。该方法在0.3 - 10μg/mg范围内对EP、0.06 - 2.5μg/mg范围内对PE和NPE以及0.04 - 1μg/mg范围内对NE和MPE进行了验证。膳食补充剂中不同分析物的平均回收率在65.7%至81.3%之间。定量限为EP 0.3μg/mg、PE 0.06μg/mg、NPE、NE和MPE 0.04μg/mg。该方法应用于分析各种含有麻黄（麻黄属植物）和刺蒴麻植物提取物的膳食补充剂，这些补充剂被宣传有助于控制体重、提高运动表现和能量。
