色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 897-903.DOI: 10.3724/SP.J.1123.2014.03044

• 技术与应用 • 上一篇    

毛细管电泳法测定水体中四环素类抗生素的基质效应及场放大进样技术的应用

李爱梅1, 黄茁2, 卢文平2, 徐中其1,3   

  1. 1. 东华大学化学化工与生物工程学院, 上海 201620;
    2. 长江水利委员会长江科学院, 湖北 武汉 430010;
    3. 生态纺织教育部重点实验室, 上海 201620
  • 收稿日期:2014-03-27 修回日期:2014-04-18 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 徐中其，E-mail：chemxzq@dhu.edu.cn
  • 基金资助:

    流域水资源与生态环境科学湖北省重点实验室开放研究基金项目（CKWV2013220/KY）；国家自然科学基金项目（51379016）.

Matrix effect and application of field-amplified sample injection in the analysis of four tetracyclines in waters by capillary electrophoresis

LI Aimei1, HUANG Zhuo2, LU Wenping2, XU Zhongqi1,3   

  1. 1. College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai 201620, China;
    2. Changjiang River Scientific Research Institute, Changjiang River Water Resources Commission, Wuhan 430010, China;
    3. Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Shanghai 201620, China
  • Received:2014-03-27 Revised:2014-04-18 Online:2014-08-08 Published:2014-08-01

PDF

421

被引次数

25

摘要：

比较了毛细管电泳（CE）和高效液相色谱（HPLC）技术对水体中4种四环素类抗生素（四环素、土霉素、金霉素及强力霉素）的分离效果。实验考察了水体的基质效应（pH值和水硬度）对分离的影响，优化了电泳条件，在压力进样模式（HDI）下，9.0 min内4种抗生素可达到基线分离，与HPLC相比，CE可以节省一半左右的分析时间。该方法具有良好的线性关系，检出限（LOD）在0.28~0.62 mg/L之间，迁移时间和峰面积的相对标准偏差（RSD）（n=6）分别为0.42%~0.56%及2.24%~2.95%；自来水和鱼塘水中加标回收率分别在96.3%~107.2%之间和87.1%~105.2%之间。此外，利用场放大电动进样（FASI）对目标物进行柱内预浓缩，检测灵敏度较HDI进样模式提高，LOD降至17.8~35.5 μg/L，迁移时间和峰面积的RSD（n=6）分别为0.85%~0.95%及1.69%~3.43%。CE具有样品前处理简单、分析速度快的特点，对环境水体中抗生素的检测具有明显的优势。

关键词: 场放大电动进样, 环境水体, 基质效应, 毛细管电泳, 四环素

Abstract:

The system abilities of two chromatographic techniques, capillary electrophoresis (CE) and high performance liquid chromatography (HPLC), were compared for the analysis of four tetracyclines (tetracycline, chlorotetracycline, oxytetracycline and doxycycline). The pH, concentration of background electrolyte (BGE) were optimized for the analysis of the standard mixture sample, meanwhile, the effects of separation voltage and water matrix (pH value and hardness) effects were investigated. In hydrodynamic injection (HDI) mode, a good quantitative linearity and baseline separation within 9.0 min were obtained for the four tetracyclines at the optimal conditions; the analytical time was about half of that of HPLC. The limits of detection (LODs) were in the range of 0.28-0.62 mg/L, and the relative standard deviations (RSDs) (n=6) of migration time and peak area were 0.42%-0.56% and 2.24%-2.95%, respectively. The obtained recoveries spiked in tap water and fishpond water were at the ranges of 96.3%-107.2% and 87.1%-105.2%, respectively. In addition, the stacking method, field-amplified sample injection (FASI), was employed to improve the sensitivity, and the LOD was down to the range of 17.8-35.5 μg/L. With FASI stacking, the RSDs (n=6) of migration time and peak area were 0.85%-0.95% and 1.69%-3.43%, respectively. Due to the advantages of simple sample pretreatment and fast speed, CE is promising in the analysis of the antibiotics in environmental water.

Key words: capillary electrophoresis (CE), environmental water, field-amplified sample injection (FASI), matrix effect, tetracyclines (TCs)

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