硅烷衍生化气相色谱法测定桑叶中1-脱氧野尻霉素含量  被引量:3

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

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作  者:王济强 张菁 

机构地区:[1]上海丝绸集团股份有限公司,上海200030

出  处:《理化检验(化学分册)》2013年第7期769-772,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基  金:国家茧丝绸发展专项资金项目(2011年度上海专项)

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×250μm,0.50μm)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。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 C for 0.5 h. The derivatized product was separated on TRB5 column (30 m×250μm, 0.50 μm), determined by FID, and detec*ed qualitmively 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%.

关 键 词:气相色谱法 1-脱氧野尻霉素 桑叶 气相色谱-质谱法 硅烷衍生化 

分 类 号:O657.7[理学—分析化学]

 

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