Dipartimento di Scienze Farmaceutiche, Università degli Studi di Milano, Via Luigi Mangiagalli 25, 20133 Milano, Italy.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jun 15;929:142-8. doi: 10.1016/j.jchromb.2013.04.012. Epub 2013 Apr 18.
The GC method previously reported by our research group for the analysis of the active principles of Catha edulis, i.e. cathine, cathinone and phenylpropanolamine, was considerably improved. N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) as derivatizing agent was employed, thus allowing an accurate determination of the analytes and a suitable internal standard for quantitative analyses (nicotinamide) was introduced. Moreover the chromatographic conditions were carefully studied to improve the separation of the alkaloids and sensitivity. To this end different chromatographic capillary columns and temperature gradients were investigated. The optimized GC method was validated and resulted adequate for the application in forensic analysis. Finally on behalf of the Tribunal, C. edulis vegetable material seized by the police in northern Italy was analyzed, the quantity of cathine ranging from 0.095 to 0.29%, the quantity of PPA from 0.010 to 0.21% and the quantity of cathinone from 0.025 to 0.374% of the weight of the vegetable material.
本研究组之前报道的用于分析卡他碱、卡西酮和苯丙醇胺等卡特叶有效成分的 GC 方法得到了显著改进。采用 N-甲基-N-三甲基硅基三氟乙酰胺(MSTFA)作为衍生化试剂,从而可以准确地测定分析物,并引入合适的内标物(烟酰胺)进行定量分析。此外,还仔细研究了色谱条件,以改善生物碱的分离度和灵敏度。为此,研究了不同的色谱毛细管柱和温度梯度。优化后的 GC 方法得到了验证,适用于法医分析。最后,代表法庭,对意大利北部警方缴获的卡特叶植物材料进行了分析,其中卡他碱的含量范围为 0.095%至 0.29%,PPA 的含量范围为 0.010%至 0.21%,卡西酮的含量范围为 0.025%至 0.374%,均为植物材料重量的百分比。