Sporkert Frank, Pragst Fritz, Bachus Rainer, Masuhr Florian, Harms Lutz
Institute of Legal Medicine, University Rostock, St.-Georg-Street 108, 18055 Rostock, Germany.
Forensic Sci Int. 2003 Apr 23;133(1-2):39-46. doi: 10.1016/s0379-0738(03)00048-3.
A sensitive and reproducible method for the quantitative determination of cathinone (CTN), norpseudoephedrine (NPE, cathine) and norephedrine (NE) from hair was developed. The compounds were extracted for 4 hours with phosphate buffer pH 2.0, followed by a standard solid phase extraction procedure on a mixed phase column, derivatization with heptafluorobutyric anhydride (HFBA) and GC-MS separation and quantification using D(3)-ephedrine (D(3)-E) and alpha-aminoacetophenone (AAP) as the internal standards. The diastereomers NPE and NE were satisfactorily separated. In the validation, the limits of detection and of quantification were determined at 0.03-0.08 ng/mg and 0.10-0.24 ng/mg, respectively and the interday standard deviation was between 10 and 15%. The method was applied to hair samples of 24 Yemenite khat chewers. All three compounds were detected in 23 of these cases. The concentrations ranged from 0.57 to 23.9 ng/mg for NPE, 0.19-25.0 ng/mg for NE and 0.11-22.7ng/mg for CTN. A highly significant correlation was found between the self-reported data about the khat consumption habits of the volunteers (4-56h chewing per week) and the concentrations of norephedrine and norpseudoephedrine in hair.
开发了一种灵敏且可重复的方法,用于定量测定毛发中的卡西酮(CTN)、去甲伪麻黄碱(NPE,去甲伪麻黄碱)和去甲麻黄碱(NE)。用pH 2.0的磷酸盐缓冲液提取这些化合物4小时,然后在混合相柱上进行标准固相萃取程序,用七氟丁酸酐(HFBA)衍生化,并使用D(3)-麻黄碱(D(3)-E)和α-氨基苯乙酮(AAP)作为内标进行气相色谱-质谱分离和定量。非对映异构体NPE和NE得到了满意的分离。在验证过程中,检测限和定量限分别确定为0.03 - 0.08 ng/mg和0.10 - 0.24 ng/mg,日间标准偏差在10%至15%之间。该方法应用于24名也门卡特叶咀嚼者的毛发样本。在其中23例中检测到了所有三种化合物。NPE的浓度范围为0.57至23.9 ng/mg,NE为0.19 - 25.0 ng/mg,CTN为0.11 - 22.7 ng/mg。在志愿者关于卡特叶消费习惯的自我报告数据(每周咀嚼4 - 56小时)与毛发中去甲麻黄碱和去甲伪麻黄碱的浓度之间发现了高度显著的相关性。