色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1199-1204.DOI: 10.3724/SP.J.1123.2011.01199

• 研究论文 • 上一篇    下一篇

中空纤维三相液相微萃取-高效液相色谱法测定环境水样中7种苯氧羧酸类除草剂

彭晓俊*, 庞晋山, 邓爱华   

  1. 新会出入境检验检疫局, 广东 江门 529100
  • 收稿日期:2011-08-01 修回日期:2011-09-23 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 彭晓俊,工程师,硕士,研究方向为理化检测和仪器分析. Tel: (0750)6312076,

Determination of seven phenoxyacid herbicides in environmental water by high performance liquid chromatography coupled with three phase hollow fiber liquid phase microextraction

PENG Xiaojun*, PANG Jinshan, DENG Aihua   

  1. Xinhui Entry-Exit Inspection and Quarantine Bureau, Jiangmen 529100, China
  • Received:2011-08-01 Revised:2011-09-23 Online:2011-12-28 Published:2012-01-15

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摘要： 建立了利用中空纤维三相液相微萃取-高效液相色谱联用技术(HF-LPME-HPLC)同时测定环境水中痕量麦草畏(dicamba)、氟草烟(fluroxypyr)、4-氯苯氧乙酸(4-CPA)、2甲4氯(MCPA)、2,4-滴(2,4-D)、2,4-滴苯氧丁酸(2,4-DB)和2甲4氯苯氧丁酸(MCPB)等7种苯氧羧酸类除草剂的分析方法。考察了萃取剂﹑接受相和给出相pH值、萃取时间﹑搅拌速度和盐效应等对检测的影响,通过正交试验优化萃取条件,得到的最佳萃取条件为正辛醇作萃取剂,给出相pH为3,接受相pH为12,萃取30 min,搅拌速度400 r/min。结果表明7种除草剂在较宽的线性范围内线性良好,相关系数为0.9953～0.9988,检出限(信噪比为3)为0.2～1.0 μg/L,富集倍数为76.7～121,加标回收率为68%～104%,相对标准偏差为3.2%～8.1%。该法灵敏度高、操作简单、检测快速、有机溶剂消耗少,为环境水样中痕量苯氧羧酸类除草剂残留的分析提供了有益的参考。

关键词: 苯氧羧酸类除草剂, 高效液相色谱, 环境水, 三相液相微萃取, 中空纤维

Abstract: A novel method for the simultaneous determination of seven phenoxyacid herbicides such as dicamba, fluroxypyr, 4-chlorophenoxyacetic acid (4-CPA), 2-methyl-4-chlorophenoxyacetic acid (MCPA), 2,4-dichlorophenoxyacetic acid (2,4-D), 2,4-dichlorophenoxybutyric acid (2,4-DB) and 4-(2-methyl-4-chlorophenoxy)butyric acid （MCPB） in environmental water by three phase hollow fiber liquid phase microextraction (HF-LPME) coupled with high performance liquid chromatography (HPLC) was developed. In order to optimize the experimental conditions, the orthogonal test has been used. The effects of extraction solvent, pH of the donor phase and acceptor phase, extraction time, stirring speed and salt concentration on the detection were investigated. The optimal experimental conditions were as follows: octanol as organic solvent, pH 3 of donor phase, pH 12 of acceptor phase, extraction time of 30 min, stirring speed of 400 r/min. The results showed that the proposed method provided a wide linear range for 7 phenoxyacid herbicides with correlation coefficients of 0.9953~0.9988. The detection limits ranged from 0.2 to 1.0 μg/L. The enrichment factors were in the range of 76.7~121. The recoveries were in the range of 68%~104% and the relative standard deviations (RSDs) were less than 8.1% for the environmental water samples. The method has the advantages of sensitivity, simplicity, fastness and the use of very small amounts of organic solvent. The method can meet the requirements of the determination of trace phenoxyacid herbicides in the environmental water samples, and the study provided a useful method for the analysis of trace substances in water samples.

Key words: environmental water, high performance liquid chromatography （HPLC）, phenoxyacid herbicides, three phase liquid phase microextraction, hollow fiber