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柱前衍生化法测定葫芦巴中4-羟基异亮氨酸的含量
引用本文:李波,曾光尧,谭健兵,周应军,谭桂山.柱前衍生化法测定葫芦巴中4-羟基异亮氨酸的含量[J].中南药学,2009,7(4):277-279.
作者姓名:李波  曾光尧  谭健兵  周应军  谭桂山
作者单位:1. 湖南省药品食品监督管理局,长沙,410013
2. 中南大学药学院,长沙,420013
摘    要:目的 建立葫芦巴中4-羟基异亮氨酸的含量测定方法。方法采用反相高效液相色谱、柱前邻苯二甲醛衍生化法。Kromasil ODS(250mm×4.6mm,5μm)色谱柱为固定相,甲醇-0.05mol·L。醋酸钠水溶液(pH=7.2,其中加入0.5%四氢呋喃)梯度洗脱(0min~20min,30:70;30min,40:60),检测波长为340nm,柱温为30c,流速为1mL·min^-1。结果4-羟基异亮氨酸在0.1848~3.696μg与峰面积呈良好的线性关系(r=0.999),平均回收率-99.12%.RSD=2.15%(n=6)。结论测定方法简便、准确,首次建立了葫芦巴药材的4-羟基异亮氨酸的邻苯二甲醛柱前衍生化含量测定方法,为葫芦巴质量控制及综合利用提供了依据。

关 键 词:葫芦巴  4-羟基异亮氨酸  反相高效液相色谱法  柱前衍生化法

Content determination of 4-hydroxyisoleucine inTriganellaj oenumgraecum L.by pre-column derivatization of HPLC
LI Bo,ZENG Guang-yao,TAN Jian-bing,ZHOU Ying-jun,TAN Gui-shan.Content determination of 4-hydroxyisoleucine inTriganellaj oenumgraecum L.by pre-column derivatization of HPLC[J].Central South Pharmacy,2009,7(4):277-279.
Authors:LI Bo  ZENG Guang-yao  TAN Jian-bing  ZHOU Ying-jun  TAN Gui-shan
Institution:1. Hunan Food and Drug Ad- ministration, Changsha 4100131 2. School of Pharmaceutical Sciences, Central South University, Changsha 410013)
Abstract:Objective To establish a method for the content determination of 4-hydroxyisoleucine in Triganellaj oenumgraecum L. Methods A pre-column derivation was developed by HPLC with o-phthaladehyde. HPLC was used with Kromasil ODS(250 mm×4.6 mm, 5μm)column, methanol-0. 5mol·L^-1 sodium acetate(0 min-20 min, 30 :70; 30 min, 40 : 60) was used as the mobile phase. The detection wavelength was 340 nm and the flow rate was 1 mL·min^-1. Results The calibration curve of 4-hydroxyisoleucine was linear at 0. 184 8~3. 696μg (r=0. 999). The average recovery was 99.12%, RSD=2.15% (n=6) . Conclusion The method is rapid, accurate and suitable for the quality control of Triganellaj oenumgraecum L.
Keywords:Triganellaj oenumgraecum L    4-hydroxyisoleucine  RP-HPLC  pre-eolumn derivation
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