硅烷衍生化气相色谱法测定桑叶中1-脱氧野尻霉素含量

GC Determination of 1-Deoxynojirimycin in Mulberry Leaves Derivatized with Silanes

摘要: 提出了用气相色谱法测定桑叶中1-脱氧野尻霉素(DNJ)含量的方法。桑叶提取液中的DNJ与六甲基二硅胺烷和三甲基氯硅烷于60 ℃加热0.5 h进行衍生反应,产物用TRB5色谱柱(30 m×250 μm,0.50 μm)分离、火焰离子化检测器定量和气相色谱-质谱法定性。DNJ的质量浓度在0.01~0.10 g·L-1范围内与峰面积呈线性关系,检出限(3S/N)为0.06 mg·L-1。应用此方法分析桑叶提取物,测定值的相对标准偏差(n=6)为1.9%,方法的回收率在101%~103%之间。

Abstract: A method of GC for the determination of 1-deoxynojirimycin(DNJ)in mulberry leaves was proposed. DNJ in the extract of mulberry leaves was derivatized with hexamethyldisilazane and trimethylchlorosilane at 60 ℃ for 0.5 h. The derivatized product was separated on TRB5 column (30 m×250 μm, 0.50 μm), determined by FID, and detected qualitatively by GC-MS. Linear relationship between values of peak area and mass concentration of DNJ was kept in the range of 0.01-0.10 g·L-1, with detection limit (3S/N) of 0.06 mg·L-1. The proposed method was applied to the analysis of extract of mulberry leaves, giving values of RSD (n=6) of 1.9%, and recovery in the range of 101%-103%.