[1]贺江,龙海波.分散液相微萃取-高效液相色谱法测定水体中毒死蜱残留[J].江苏农业学报,2015,(05):1179-1183.[doi:doi:10.3969/j.issn.1000-4440.2015.05.037]
 HE Jiang,LONG Hai-bo.A dispersive liquid-liquid microextraction-HPLC method for determination of chlorpyrifos in water[J].,2015,(05):1179-1183.[doi:doi:10.3969/j.issn.1000-4440.2015.05.037]
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分散液相微萃取-高效液相色谱法测定水体中毒死蜱残留()
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江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2015年05期
页码:
1179-1183
栏目:
加工贮藏·质量安全
出版日期:
2015-10-31

文章信息/Info

Title:
A dispersive liquid-liquid microextraction-HPLC method for determination of chlorpyrifos in water
作者:
贺江龙海波
(湖南文理学院 生命科学学院, 环洞庭湖水产健康养殖与加工湖南省重点实验室, 湖南省水产高效健康生产协同创新中心, 湖南常德415000)
Author(s):
HE JiangLONG Hai-bo
(College of Life Science, Hunan University of Art and Science/Hunan Provincial Key Laboratory of Aquatic Healthy Farming and Processing in Dongting Lake/ Collaborative Innovation Center for Efficient and Healthy Production of Fisheries in Hunan Province, Changde 415000,China)
关键词:
分散液相微萃取高效液相色谱毒死蜱水体农药残留
Keywords:
dispersive liquid-liquid micro extractionhigh performance liquid chromatographychlorpyrifoswaterpesticide residue
分类号:
S132
DOI:
doi:10.3969/j.issn.1000-4440.2015.05.037
文献标志码:
A
摘要:
水体中的农药残留是严重的环境安全问题之一,并可通过水产养殖或种植业等途径污染食品。本研究应用分散液相微萃取(Dispersive liquid-liquid microextraction ,DLLME)技术,建立水体中毒死蜱的高效液相色谱(High performance liquid chromatography ,HPLC)分析方法。通过考察萃取剂种类、分散剂种类、萃取剂用量、分散剂用量、盐度以及pH等因素对分散液相微萃取的影响,确定最佳操作参数。经优化的水体中毒死蜱分散液相微萃取过程为:以100 μl三氯乙烷为萃取剂,1 200 μl甲醇为分散剂,混匀后,加入10 ml水样,室温静置2 min,以3 000 r/min离心2 min,吸取15 μl沉积相,进行HPLC分析。本方法操作简单、成本低,灵敏度、准确度及精密度高,可为水体中毒死蜱残留检测提供新的方法。
Abstract:
The residue of pesticides in water system is one of the serious environmental safety problems, and may contaminate food through a variety of ways. In the current study, dispersive liquid-liquid micro-extraction (DLLME) technology was applied for develop a high performance liquid chromatography (HPLC) analysis methods for the detection of chlorpyrifos in water. In the optimized protocol, the mixture of 100 μl trichloroethane used as extract agent and 1 200 μl methanol used as dispersing agent were added with 10.0 ml water samples and stored at room temperature for 2 min, and 15 μl deposition sampled from above mixture centrifuged at 3 000  r/min for 2 min were subjected to HPLC analysis. The newly developed method was applied to detected the chlorpyrifos with the concentrations ranging from 0.01~1.00 mg/L, the results showed the spiked recoveryes were above 85.5%, indicative of the sensitivity, accuracy and precision. This method offers a new approch for the detection of chlorpyrifos in water sample.〖JP〗

参考文献/References:

[1]和晓彤. 农药残留分析前处理技术研究进展[J]. 广东农业科学, 2011(17): 132-135.
[2]牛鹏飞,仇农学,郭玉蓉,等. 固相萃取结合高效液相色谱同时检测浓缩苹果汁中6种农药残留[J]. 江苏农业学报, 2010, 26(4): 843-847.
[3]ZHAO C L, DING R Y, HUO L G, et al. Determination of pesticide residues in tea by gas chromatography / triple quadrupole mass spectrometry with solid-phase extraction[J]. J AOAC Int,2014, 97(4): 1001-1006.
[4]张艳,王松雪,孙长坡. 超临界流体萃取技术在粮食农药残留检测中的应用[J]. 食品科学, 2010, 31(1): 274-277.
[5]CHIKUSHI H, HIROTA K, YOSHIDA N, et al. Simple water analysis of golf link pesticides by means of batch-wise adsorption and supercritical fluid extraction[J]. Talanta, 2009, 80(2): 738-743.
[6]罗美中,李苑雯,陈素娟,等. 固相微萃取-气相色谱-质谱法同时测定天然饮用水中39种有机污染物[J]. 理化检验:化学分册, 2013, 49(3): 329-333.
[7]BASHEER C, ALNEDHARY A A, RAO B S, et al. Determination of carbamate pesticides using micro-solid-phase extraction combined with high-performance liquid chromatography[J]. J Chromatogr A,2009, 16(2): 211-216.
[8]李星星,汪路路,孙福生. 基于离子液体的单滴液相微萃取-高效液相色谱法测定水中杀螨隆农药残留[J]. 分析试验室, 2011, 30(3): 73-76.
[9]TSIROPOULOS N G, AMVRAZI E G. Determination of pesticide residues in honey by single-drop microextraction and gas chromatography[J]. J AOAC Int, 2011, 94(2): 634-644.
[10]GONZLEZ-CURBELO M , HERNNDEZ-BORGES J, BORGES-MIQUEL T M, et al. Determination of organophosphorus pesticides and metabolites in cereal-based baby foods and wheat flour by means of ultrasound-assisted extraction and hollow-fiber liquid-phase microextraction prior to gas chromatography with nitrogen phosphorus detection[J]. J Chromatogr A, 2013, 1313: 166-174.
[11]张雪莲,焦必宁. 分散液液微萃取技术及其在食品和环境农药残留检测中的应用[J]. 食品科学, 2012, 33(9): 307-313.
[12]苗雪雪,杨愿愿,刘登彪,等. 分散液液微萃取-气质联用法测定牛奶中酰胺类除草剂[J]. 华南农业大学学报, 2015, 36(2): 43-48.
[13]侯德坤,何江,张福金,等. 分散液-液微萃取技术在污染物分析中的应用[J]. 分析测试学报, 2014, 33(5): 606-614.
[14]WU Q, ZHOU X, LI Y, et al. Application of dispersive liquid–liquid microextraction combined with high-performance liquid chromatography to the determination of carbamate pesticides in water samples[J]. Anal Bioanal Chem, 2009, 393: 1755-1761.
[15]韩畅,朱鲁生,王军,等. HPLC测定水体中毒死蜱及其有毒降解产物TCP[J]. 农业环境科学学报, 2009, 28(7): 1552-1556.〖ZK)〗〖FL)〗

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备注/Memo

备注/Memo:
收稿日期:2015-03-20 基金项目:国家自然科学基金项目(31401583);湖南省教育厅科研项目(12C0828);湖南省常德市联合基金项目(2015JJ5008);湖南文理学院生命科学学院省级平台开放项目(SKYPT201202) 作者简介:贺江(1983-),男,江西萍乡人,博士,讲师,主要从事食品安全与食品生物技术方面的研究。(Tel)15115667084;(E-mail) hejiang1119@163.com
更新日期/Last Update: 2015-10-31