钩吻素甲的气相色谱-质谱分析

Determination of Gelsemine by Gas ChromatograpHy-Mass Spectrometry

取 5 g生物组织绞成均浆状 ,用甲醇、水和盐酸混合液进行溶解和液 -液提取生物碱中的钩吻素甲。用急速升温法减少了样品中杂质对色谱 -质谱测量的影响。在最优化的 GC/ MS条件下获得了钩吻素甲的主要特征峰为 m/ z1 0 8(基峰 )、m/ z2 5 1、m/ z2 79和 m/ z3 2 2 (分子离子 M+ 峰 )。由此确定了钩吻素甲的分子式C2 0 H2 2 N2 O2 、分子量 3 2 2 Da和分子结构。

Biological tissue was weighed 5g, and was whisked to become the jam-like and was prepared the solution sample with use of the mixture of methanol, water and hydrochlororic acid. Gelsemine was extracted from the solution sample by liquid-liquid extractive method. The effect of the impurity in biological sample for the gas chromatography-mass spectrometry (GC/MS) measuring was minimized by fast rising temperature. The main characteristic peaks m/z108(basic peak), m/z251, m/z279 and m/z322(M +) were detected by the selective ion monitoring (SIM) mode under the optimizing GC/MS parameters. Therefore, the molecular formula(C 20H 22N 2O 2), molecular weight (322Da) and molecular structure were determinated. Therewith, a extraction and analysis method of this poison was found for the judicial identify.