色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1210-1215.DOI: 10.3724/SP.J.1123.2011.01210

• 研究论文 • 上一篇    下一篇

高效液相色谱法考察 60Co-γ射线照射天麻其化学成分的稳定性

杨孝容1*, 黄敏2, 刘素君1, 宋九华1   

  1. 1. 乐山师范学院化学与生命科学学院, 四川 乐山 614004; 2. 四川省原子能研究院, 四川 成都 610101
  • 收稿日期:2011-08-25 修回日期:2011-10-31 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 杨孝容,教授,主要研究方向为色谱和光谱分析.
  • 基金资助:

    四川省科技支撑计划项目(2009sz127).

Stability evaluation of chemical compositions of Rhizoma gastrodiae with 60Co-γ irradiation by high performance liquid chromatography

YANG Xiaorong1*, HUANG Min2, LIU Sujun1, SONG Jiuhua1   

  1. 1. College of Chemistry and Life Sciences, Leshan Normal University, Leshan 614004, China; 2. Sichuan Institute of Atomic Energy, Chengdu 610101, China
  • Received:2011-08-25 Revised:2011-10-31 Online:2011-12-28 Published:2012-01-15

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摘要： 建立了快速检测大鼠血浆中普萘洛尔对映体浓度的柱切换-高效液相色谱法。将自制限进填料柱作为预处理柱,通过直接进样方式,使普萘洛尔对映体在预处理柱上保留,同时除去血浆中的蛋白质等大分子;再通过柱切换技术,使普萘洛尔对映体在键合型纤维素-三(3,5-二甲基苯基氨基甲酸酯)(Chiralcel OD-RH)分析柱上得到手性拆分。通过条件优化,确定切换前预处理流动相为硼酸盐缓冲液(pH 8.5)-甲醇(95:5, v/v),流速为1.0 mL/min;切换后分析流动相为异丙醇-乙醇-0.2 mmol/L硼酸盐缓冲液(pH 8.5)(30:30:40, v/v/v),流速为0.8 mL/min;切换时间为3 min;柱温为25 ℃;检测波长为293 nm。普萘洛尔两对映体在25～500 mg/L的质量浓度范围内具有良好的线性关系(r=0.9995), 3个加标水平(50、100、250 mg/L)的平均回收率为97.89%～101.56%,日内和日间精密度均小于5%。该方法简便、快速、灵敏、准确,适于血浆样本中手性药物的药代动力学研究。

关键词: 60Co-γ照射, 高效液相色谱, 天麻, 稳定性, 主要指纹峰

Abstract: The main chromatographic fingerprint peaks of Rhizoma gastrodiae were established for evaluating the stability of chemical compositions of Rhizoma gastrodiae with 60Co-γ irradiation to control the dosage of 60Co-γ irradiation sterilization by high performance liquid chromatography (HPLC). Eight Rhizoma gastrodiae samples were analyzed. The chromatographic fingerprints of Rhizoma gastrodiae were constructed with 14 common fingerprint peaks, and its 10 main peaks were identified using the similarity evaluation system of chromatographic fingerprints of traditional Chinese medicine (version 2004 A) recommended by State Food and Drug Administration of China. The relative standard deviations of the peak areas of the 10 main peaks were used to evaluate the stability of corresponding chemical compositions of Rhizoma gastrodiae with 60Co-γ irradiation. The results showed that the compositions of 3 of the 10 main peaks were influenced and a good relationship was obtained between the influence and 60Co-γ irradiation doses for the eight Rhizoma gastrodiae samples. Some chemical components of Rhizoma gastrodiae weren’t steady after 60Co-γ irradiation, so a low dosage should be selected for 60Co-γ irradiation sterilization.

Key words: 60Co-&gamma, Rhizoma gastrodiae, stability, high performance liquid chromatography (HPLC), irradiation, main fingerprint peak