色谱 ›› 2018, Vol. 36 ›› Issue (7): 665-669.DOI: 10.3724/SP.J.1123.2018.02003

• 研究论文 • 上一篇    下一篇

气泡富集-高效液相色谱法测定地表水样中微量土霉素

熊方永, 蔡云枫, 张英, 丁健桦   

  1. 东华理工大学化学生物与材料科学学院, 江西 南昌 330013
  • 收稿日期:2018-01-08 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 丁健桦,E-mail:dingjianh2004@126.com
  • 基金资助:

    长江学者和创新团队发展计划项目(IRT_17R20);高等学校学科创新引智计划(111计划)(D17006);江西省对外科技合作计划项目(20161BBH80055).

Determination of trace amounts of oxytetracycline in surface water samples by bubble enrichment-high performance liquid chromatography

XIONG Fangyong, CAI Yunfeng, ZHANG Ying, DING Jianhua   

  1. Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, East China University of Technology, Nanchang 330013 China
  • Received:2018-01-08 Online:2018-07-08 Published:2014-06-03
  • Supported by:

    Program for Changjiang Scholars and Innovative Research Team in University(PCSIRT)(No. IRT_17R20);the 111 Project(No. D17006);Jiangxi Province Foreign Science and Technology Cooperation Project(No. 20161BBH80055).

摘要:

建立了气泡富集-高效液相色谱(HPLC)测定地表水样中微量土霉素的方法。采用新型样品前处理方法——气泡富集法,对水溶液中的微量土霉素进行富集,考察了气泡富集条件对富集效果的影响。研究发现,在优化的气泡富集和色谱条件下,土霉素的富集倍数可达37.06,土霉素含量测定的RSD为4.8%(n=11),LOD为0.038 mg/L。将该方法用于地表水样中土霉素的测定,平均加标回收率为101.9%。可见,气泡富集法对土霉素的富集效果好,能与色谱结合用于地表水样中土霉素的快速、灵敏、准确检测。同时,在进行样品前处理时无需任何有机溶剂,而且装置简单、成本低廉、易操作。可见气泡富集法是一种非常有研究和推广价值的绿色样品前处理方法,有望用于复杂样品中其他微量甚至痕量物质的分析。

关键词: 地表水, 高效液相色谱, 气泡富集法, 土霉素

Abstract:

A method was established to determine the trace amounts of oxytetracycline (OTC) in surface water samples by bubble enrichment-high performance liquid chromatography (HPLC). A novel sample pretreatment method, bubble enrichment, was used to enrich trace amounts of oxytetracycline in aqueous solutions, and the effects of bubble enrichment conditions on the enrichment efficiency was investigated. Enrichment factor of oxytetracycline had a maximum of 37.06, RSD was 4.8% (n=11), and LOD was 0.038 mg/L under the optimized conditions of bubble enrichment and chromatography. The method was applied to the determination of oxytetracycline in surface water samples, with an average recovery of 101.9%. It is obvious that bubble enrichment has a positive effect on the enrichment of oxytetracycline, and hence, can be combined with chromatography to realize rapid, sensitive, and accurate detection of oxytetracycline in surface water samples. Additionally, the bubble enrichment method used in this paper does not require any organic solvent for the pretreatment of samples, and furthermore, the device is simple, inexpensive, and easy to operate; therefore, it is a very green sample pretreatment method with great research and promotion value. It is expected to be applicable to the analysis of other trace substances in complex samples.

Key words: bubble enrichment, high performance liquid chromatography(HPLC), oxytetracycline(OTC), surface water

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