色谱

色谱

• 研究论文 • 上一篇    下一篇

反相高效液相色谱-蒸发光散射检测法同时测定阿胶中的17种未衍生氨基酸

鄢丹1,2,韩玉梅1,2,董小萍2

  

  1. 1.Institute of Chinese Medicine, 302 Hospital of People’s Liberation Army, Beijing 100039, China;
    2.Chengdu University of Traditional Chinese Medicine, Chengdu 610075, China

  • 收稿日期:2005-09-05 修回日期:2005-10-31 出版日期:2006-07-30 发布日期:1986-12-25
  • 通讯作者: 鄢丹

Simultaneous Determination of 17 Underivatized Amino Acids in Donkey-Hide Glue by Reversed-Phase
High Performance Liquid Chromatography-Evaporative Light-Scattering Detection

YAN Dan1,2, HAN Yumei1,2, DONG Xiaoping2

  

  1. 1.Institute of Chinese Medicine, 302 Hospital of People’s Liberation Army, Beijing 100039, China;
    2.Chengdu University of Traditional Chinese Medicine, Chengdu 610075, China

  • Received:2005-09-05 Revised:2005-10-31 Online:2006-07-30 Published:1986-12-25
  • Contact: YAN Dan

PDF

1351

摘要：

建立了反相高效液相色谱-蒸发光散射检测法(HPLC-ELSD)同时测定中药阿胶中17种未衍生氨基酸含量的方法。采
用PrevailTMC18色谱柱 (250 mm×4.6 mm i.d., 5 μm)，以乙腈-0.7%三氟醋酸溶液(含5.0 mmol/L七氟丁酸）为流
动相进行线性梯度洗脱，流速为0.8 mL/min，在漂移管温度115 ℃、氮气流量2.5 L/min条件下，在25 min内即可完成
对阿胶中17种氨基酸的分离测定。氨基酸质量浓度为0.073～2.327 g/L时,其峰面积的对数值与质量浓度的对数值线性
关系良好；17种氨基酸的加样回收率为93.5%～104.8%；信噪比为3时,测得氨基酸的最低检测限介于18.2 mg/L与54.6
mg/L之间。该法快速、简便、准确,可作为阿胶中氨基酸的直接测定方法,亦为其他药物中氨基酸的分析提供了参考。

关键词: 阿胶 , 氨基酸, 反相高效液相色谱, 未衍生化, 蒸发光散射检测

Abstract:

An analytical method to determine 17 underivatized amino acids in donkey-hide glue was
established with reversed-phase high performance liquid chromatography (HPLC) coupled with
evaporative light-scattering detection (ELSD). A PrevailTM C18 column was used with the mobile phase
of acetonitrile-0.7% trifluoroacetic acid containing 5.0 mmol/L heptafluorobutyric acid. Under the
condition of solvent gradient elution, the temperature of drift tube was 115 ℃ and the gas flow
rate was 2.5 L/min. The 17 amino acids were separated within 25 min. The good linearities between
the logarithm of peak area and logarithm of mass concentration of amino acids were obtained in a
range of mass concentrations from 0.073 g/L to 2.327 g/L. The recoveries of 17 amino acids were
93.5%-104.8% with the relative standard deviations (RSDs) of 0.58%-2.88%. The lowest detection
limits of amino acids were from 18.2 mg/L to 54.6 mg/L with 3 times the signal to noise ratio.
This HPLC-ELSD method is rapid, simple and accurate. It can be used for the direct determination of
17 underivatized amino acids in donkey-hide glue. It also serves as a good reference for the
determination of amino acids in other fields, such as pharmaceutical analysis.

Key words: amino acid, donkey-hide glue , evaporative
light-scattering detection (ELSD), underivatized, reversed-phase high performance liquid chromatography (RP-HPLC)