高效液相色谱法测定金糖宁胶囊中1-脱氧野尻霉素的含量  

Determination of 1-Deoxynojirimycin in Jintangning Capsules by HPLC

作　　者：于娟 杜守颖[2] 吴丽璇 陈啟兰 

机构地区：[1]漳州片仔癀药业股份有限公司,福建漳州363000 [2]北京中医药大学,北京100029

出　　处：《中国实验方剂学杂志》2015年第18期62-64,共3页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：福建省科技重大专项(2006YZ0001-4)

摘　　要：目的：建立反相高效液相色谱-柱前衍生化法测定金糖宁胶囊中1-脱氧野尻霉素（1-DNJ）的含量。方法：样品经处理过的D001-CC型阳离子交换树脂上用氨水洗脱收集后,用2 g·L^-1的芴甲氧羰酰氯（FMOC-C1）柱前衍生化,再采用高效液相色谱-二极管阵列检测器测定。ODS-C18色谱柱（4.0 mm×250 mm,5μm）,流动相乙睛-0.2%磷酸溶液梯度洗脱,流速1.0 m L·min^-1,检测波长263 nm,柱温25℃。结果：1-脱氧野尻霉素在0.84-8.4μg线性关系良好（r=1.000 0）,精密度RSD0.3%,重复性RSD 0.6%,衍生化后的样品溶液在24 h内稳定,平均回收率109.6%,RSD 0.4%。结论：该方法稳定可靠,重复性好,精密度高,可用于金糖宁胶囊中1-脱氧野尻霉素的含量测定。Objective ： To develop a HPLC method of determination of 1-deoxynojirimycin in Jintangning capsules. Method： The samples were collected after elution with ammonia by processed D001-CC type positive cation exchange resin and pre-column derivatization with the concentration of 2 g · L^-1 of 9-fluorenylmethyl chloroformate （Fmoc-C1） and then determinated by DAD detector. ODS-C18 （4.0 mm ×250 mm, 5μm） was eluted with the mobile phase of acetonitrile and 0.2% phosphoric acid in a gradient mode. The flow rate was 1.0 mL .min-~, the detection wavelength was 263 nm, and column temperature at 25℃. Result： 1-deoxynojirimycin had good linear relationships within the range of 0. 84-8.4 μg （r = 1. 000 0） , with the precision RSD of 0.3% and repetition RSD of 0.6% , the sample solution after derivatization was stable within 24 hours. The average recovery was 109.6% , and the relative standard deviations were 0. 4%. Conclusion： The method is stable, reliable and accurate, and can be used for the determination of 1-deoxynojirimycin in Jintangning capsules.

关 键 词：1-脱氧野尻霉素 金糖宁胶囊 柱前衍生化 反相高效液相色谱法 

分 类 号：R284.1[医药卫生—中药学]