色谱

色谱 ›› 2018, Vol. 36 ›› Issue (11): 1167-1172.DOI: 10.3724/SP.J.1123.2018.07018

• 研究论文 • 上一篇    下一篇

高效液相色谱法同时测定水体中氧氟沙星及其手性异构体

仲小飞1,2, 秦晓鹏1, 杜平1, 陈娟1, 张云慧1, 何赢1, 刘菲2   

  1. 1. 环境基准与风险评估国家重点实验室, 土壤与固体废物研究所, 中国环境科学研究院, 北京 100012;
    2. 水资源与环境工程北京市重点实验室, 中国地质大学(北京), 北京 100083
  • 收稿日期:2018-07-18 出版日期:2018-11-08 发布日期:2014-09-30
  • 通讯作者: 刘菲.E-mail:feiliu@cugb.edu.cn.
  • 基金资助:

    国家自然科学基金项目（41602259，41731282）.

Simultaneous determination of ofloxacin enantiomers in water by high performance liquid chromatography

ZHONG Xiaofei1,2, QIN Xiaopeng1, DU Ping1, CHEN Juan1, ZHANG Yunhui1, HE Ying1, LIU Fei2   

  1. 1. State Key Laboratory of Environmental Criteria and Risk Assessment, Institute of Soil and Solid, Chinese Research Academy of Environmental Sciences, Beijing 100012, China;
    2. Beijing Key Laboratory of Water Resources and Environmental Engineering, China University of Geosciences(Beijing), Beijing 100083, China
  • Received:2018-07-18 Online:2018-11-08 Published:2014-09-30
  • Supported by:

    National Natural Science Foundation of China (Nos. 41602259, 41731282).

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摘要：

建立了一种简单快捷的手性配位交换高效液相色谱测定地表水中氧氟沙星及其手性异构体的方法，并研究了常见金属阳离子（Ca2+、Mg2+、Fe3+、Zn2+）和腐殖酸（HA）对二者分离的影响。采用C18色谱柱（25 cm×0.46 cm，5 μm），流动相为pH值4.5的20%（v/v）甲醇水溶液（含4 mmol/L异亮氨酸（配体）和3 mmol/L CuSO4），流速为1.0 mL/min，柱温为40℃，检测波长为293 nm。氧氟沙星及其手性异构体左氧氟沙星可在18 min内分离，分离度（R）为2.70。结果表明，不同金属阳离子和腐殖酸对手性分离未见明显影响，但会降低氧氟沙星及其手性异构体的峰面积，其中Fe3+和高浓度腐殖酸的影响最大。该法能够快速高效测定地表水中氧氟沙星及其手性异构体，但在测试中需考虑Fe3+和高浓度腐殖酸的影响。

关键词: 腐殖酸, 高效液相色谱, 配位交换, 手性异构体, 阳离子, 氧氟沙星, 左氧氟沙星

Abstract:

A simple and rapid method was developed for the analysis of ofloxacin enantiomers by chiral ligand exchange-high performance liquid chromatography (CLE-HPLC). In addition, the influences of common cations (Ca2+, Mg2+, Fe3+, Zn2+) and the content of humic acid (HA) on the separation were investigated. The separation was carried out on a C18 column (25 cm×0.46 cm, 5 μm). The mobile phase was 20% (v/v) methanol aqueous solution containing 4 mmol/L L-isoleucine (as ligand) and 3 mmol/L CuSO4. The pH of the mobile phase was 4.5, and the flow rate was 1.0 mL/min. The column temperature was 40℃, and the detection wavelength was 293 nm. The ofloxacin enantiomers (ofloxacin and levofloxacin) were separated within 18 min and the resolution (R) was 2.70. The results showed that metal cations and HA had no significant influence on the resolution of ofloxacin enantiomers. However, the measured peak area of ofloxacin enantiomers decreased particularly in presence of Fe3+ and on increasing HA content. The proposed method can rapidly and efficiently determine ofloxacin and its chiral isomers in surface water, the influences of Fe3+ and HA content should be considered for verifying the applicability of the method.

Key words: cations, enantiomers, high performance liquid chromatography (HPLC), humic acid (HA), levofloxacin (LEV), ligand exchange, ofloxacin (OFL)

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