色谱

色谱

• 研究论文 • 上一篇    下一篇

中空纤维液相微萃取-高效液相色谱法测定水中残留的氨基甲酸酯类农药

杨秀敏,王志,王春,韩丹丹,陈永艳,宋双居

  

  1. Key Laboratory of Bioinorganic Chemistry, College of Science, Agricultural
    University of Hebei, Baoding 071001, China
  • 收稿日期:2006-10-31 修回日期:2006-12-25 出版日期:2007-05-30 发布日期:1985-09-25
  • 通讯作者: 王 志

Determination of Carbamate Pesticides in Reservoir Water by Hollow Fiber-Based Liquid Phase Microextraction Coupled
with High Performance Liquid Chromatography

YANG Xiumin, WANG Zhi, WANG Chun, HAN Dandan, CHEN Yongyan, SONG Shuangju   

  1. Key Laboratory of Bioinorganic Chemistry, College of Science, Agricultural
    University of Hebei, Baoding 071001, China
  • Received:2006-10-31 Revised:2006-12-25 Online:2007-05-30 Published:1985-09-25

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摘要：

应用中空纤维液相微萃取(HP-LPME)技术建立了水样中呋喃丹、西维因、异丙威和乙霉威的高效液相色谱分析方法。对影响HP-LPME的实验条件进行了优化。采用Accurel Q3/2聚丙烯中空纤维,以甲苯为萃取溶剂,于室温、搅拌速度为720 r/min条件下在4.5 mL样品溶液中萃取20 min,萃取物在室温下经氮气流吹干后用流动相溶解进样。采用Baseline C18分离柱(4.6 mm×250 mm,5.0 μm),以甲醇-水(体积比为60∶40) 为流动相，流速为1.0 mL/min。呋喃丹、西维因、异丙威和乙霉威的检测波长分别为200，223，200和208 nm。该方法对4种氨基甲酸酯类农药的富集倍数均大于45倍；4种氨基甲酸酯类农药在10~100 μg/L质量浓度范围内，其质量浓度与峰面积之间有良好的线性关系,相关系数均大于0.99；呋喃丹、西维因、异丙威和乙霉威的检出限(S/N=3)分别为5，1，5和3 μg/L；实际水样中的加标回收率为82.0%~102.2%,相对标准偏差为2.0%～6.2%(n=6)。

关键词: 氨基甲酸酯类农药, 高效液相色谱法, 水样 , 液相微萃取, 中空纤维

Abstract:

An analytical method for the determination of carbamate pesticides (carbofuran, carbaryl, isoprocarb and diethofencarb) in reservoir water using hollow fiber-based liquid phase microextraction (HF-LPME) coupled with high performance liquid chromatography (HPLC) was developed. Some main experimental parameters that affect the extraction efficiency were optimized. Toluene was selected as both the extraction solvent and the impregnation solvent. The extraction was carried out at room temperature (20 ℃) in a 5 mL Teflon-lined septum cap vial filled with 4.5 mL of sample solution at a stirring rate of 720 r/min for 20 min. The extract was dried under nitrogen stream at room temperature. The dried residue was then dissolved in the mobile phase for HPLC analysis. The separation was carried out on a Baseline C18 column (4.6 mm×250 mm, 5.0 μm) with methanol-water (60∶40, v/v) as the mobile phase at a flow rate of 1.0 mL/min. The detection for carbofuran, carbaryl, isoprocarb and diethofencarb was selected at 200, 223, 200 and 208 nm, respectively. The average enrichment factors for the four analytes were greater than 45. The linear range for the quantification of the four analytes was 10-100 μg/L （r＞0.99）. The limits of detection (LODs) were 5, 1, 5 and 3 μg/L (S/N=3) for carbofuran, carbaryl, isoprocarb and diethofencarb, respectively. Good recoveries (82.0%-102.2%) and good reproducibilities (2.0%-6.2%, n=6) were achieved.

Key words: carbamate pesticides, high performance liquid chromatography (HPLC), liquid phase microextraction, reservior water , hollow fiber