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采用气相色谱-电子电离源/负离子化学电离源质谱法(GC-EI/NCIMS)鉴定和相对定量测定烟草中4种苯丙烷类葡萄糖苷。烟样经甲醇提取,XAD-2大孔树脂柱净化,得到初步纯化的糖苷。将初提物糖苷进行酶水解或三氟乙酰化衍生,GC-EI/NCI-MS测定衍生化产物。酶解得到4种苯丙烷类糖苷配基。对三氟乙酰化EI-MS和NCI-MS解析,并结合酶解结果,获得4种苯丙烷类葡萄糖苷的准确结构。对三氟乙酰化GC-EI-MS相对定量方法进行重复性验证,结果表明,方法能较好的对其相对定量。为应用GC-MS分析缺乏标准品的糖苷物质奠定了基础。
Gas chromatography-electron ionization / anion chemical ionization mass spectrometry (GC-EI / NCIMS) was used to identify and quantify four phenylpropanoid glucosides in tobacco. The tobacco samples were extracted by methanol and purified by XAD-2 macroporous resin column to obtain the initially purified glycosides. The crude glycosides were enzymatically hydrolyzed or trifluoroacetylated, and the derivatized products were determined by GC-EI / NCI-MS. Enzymatic hydrolysis of four phenylpropanoid aglycone. The analytical results of trifluoroacetylated EI-MS and NCI-MS, combined with the results of enzymatic hydrolysis, gave the accurate structures of four phenylpropanoid glucosides. Repeated validation of the relative quantification of trifluoroacetylated GC-EI-MS showed that the method was relatively accurate. It laid the foundation for GC-MS analysis of glycoside lacking standards.