色谱 ›› 2015, Vol. 33 ›› Issue (8): 849-855.DOI: 10.3724/SP.J.1123.2015.03030

• 研究论文 • 上一篇    下一篇

整体柱在线固相微萃取-高效液相色谱同步富集检测水中的苯氧羧酸类除草剂

王家斌, 吴芳玲, 赵琦   

  1. 福州大学生物和医药技术研究院, 福建 福州 350002
  • 收稿日期:2015-03-23 出版日期:2015-08-08 发布日期:2015-07-27
  • 通讯作者: 王家斌
  • 基金资助:

    国家自然科学基金青年基金项目(31401609).

Synchronous extraction and determination of phenoxy acid herbicides in water by on-line monolithic solid phase microextraction-high performance liquid chromatography

WANG Jiabin, WU Fangling, ZHAO Qi   

  1. Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou 350002, China
  • Received:2015-03-23 Online:2015-08-08 Published:2015-07-27

摘要:

采用C18毛细管整体柱作为固相微萃取整体柱,构建在线固相微萃取-高效液相色谱联用系统,同步富集检测环境水样中的5种苯氧羧酸类除草剂。详细考察了联用系统运行条件对富集检测的影响。联用系统运行最佳参数为:固相微萃取整体柱长度20 cm,进样流速0.04 mL/min,进样13 min,洗脱流速0.02 mL/min,洗脱5 min。在最佳条件下,5种苯氧羧酸类除草剂的检出限为:9 μg/L (苯氧丙酸)、4 μg/L (2-(2-氯)-苯氧丙酸)、4 μg/L (2-(3-氯)-苯氧丙酸)、5 μg/L (2,4-二氯苯氧乙酸)、5 μg/L (2-(2,4-二氯苯氧基)丙酸)。与HPLC系统直接进样对比,联用系统对5种检测对象表现出优良的富集能力。5种苯氧羧酸类除草剂的回收率在79.0%~98.0%之间(RSD≤3.9%)。该方法成功应用于水样中5种苯氧羧酸类除草剂的检测,结果令人满意。

关键词: 苯氧羧酸类除草剂, 高效液相色谱, 同步富集检测, 在线固相微萃取, 整体柱

Abstract:

A C18 monolithic capillary column was utilized as the solid phase microextraction column to construct an in-tube SPME-HPLC system which was used to simultaneously extract and detect five phenoxy acid herbicides, including 2,4-dichlorophenoxyacetic acid (2,4-D), 2-(2-chloro)-phenoxy propionic acid (2,2-CPPA), 2-(3-chloro)-phenoxy propionic acid (2,3-CPPA), phenoxy propionic acid (PPA) and 2-(2,4-dichlorophenoxy)propionic acid (2,4-DP). The operating parameters of the in-tube SPME-HPLC system, including the length of the monolithic column, the sampling flow rate, the sampling time, the elution flow rate and the elution time, had been investigated in detail. The optimized operating parameters of the in-tube SPME-HPLC system were as follow: the length of the monolithic column was 20 cm, the sampling flow rate was 0.04 mL/min, sampling time was 13 min; the elution flow rate was 0.02 mL/min, elution time was 5 min. Under the optimized conditions, the detection limits of the five phenoxy acid herbicides were as follows: 9 μg/L for PPA, 4 μg/L for 2,2-CPPA, 4 μg/L for 2,3-CPPA, 5 μg/L for 2,4-D, 5 μg/L for 2,4-DP. Compared with the HPLC method with direct injection, the combined system showed a good enrichment factors to the analytes. The recoveries of the five phenoxy acid herbicides were between 79.0% and 98.0% (RSD≤3.9%). This method was successfully used to detect the five phenoxy acid herbicides in water samples with satisfactory results.

Key words: high performance liquid chromatography (HPLC), monolithic column, on-line solid phase microextraction, phenoxy acid herbicides, synchronous extraction and determination

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