【摘要】 建立了2,4-二硝基氟苯(DNFB)柱前荧光衍生-高效液相色谱法测定桑叶中1-脱氧野尻霉素(DNJ)的方法。桑叶干粉经索式提取器除去部分色素后加入0.1%的冰醋酸甲醇溶液,在水浴超声条件下(50°C,5min)重复提取2次,活性炭脱色后用DNFB进行衍生,DNJ反应生成荧光产物,然后用高效液相-紫外检测器测定。流动相为乙腈-0.1%醋酸甲醇(25∶75,V/V),流速1.0 mL/min,柱温10℃。线性范围为0.16~8.14μg/mL,(相关系数r=0.9994),检出限为0.03μg/mL。试验测得桑叶中DNJ的平均含量为0.30%,平均回收率为96.8%,RSD为2.0%(n=6)。更多还原

【Abstract】 A rapid and reliable method has been developed,suitable for assays of a large number of mulberry leaf for 1-deoxynojirimycin(DNJ). Dried leaf was extracted with fresh chloroform in Soxhlet extractor to remove pigments,and then DNJ in the dried leaf was double-extracted in 0.1 % acetic acid in methanol,assisted by ultrasound for 5 min at 50 ℃ for each time.After that active carbon was used to the pooled extract and vortexed for 30 s to remove residual pigments.Finally,the extract was derivatized with 2,4-Dinitro-1-fluorobenzene(DNFB),and analyzed by high performance liquid chromatography equipped with ultraviolet detector.Mobile phase consisted of acetonitrile-0.1% acetic acid in methanol(25∶75,V/V) with a flow rate of 1.0 mL/min.The linear calibration curve was established with the concentration range from 0.16 μg/ mL to 8.14 μg/mL,r = 0.9994 of the correlation coefficient,and 0.03 μg/mL (3σ) of the detective limit.The results showed that the content of DNJ in leaf of Morus alba L.was 0.30%,the average recovery was 96.8%,and RSD was 2.0%(n=6).更多还原