气相色谱法测定水产品中的氟乐灵

食品科学 ›› 2012, Vol. 33 ›› Issue (22): 214-216.

气相色谱法测定水产品中的氟乐灵

刘慧慧1,2，任传博3，宫向红1,2，徐英江1,2，邓旭修3，张华威3，田秀慧1,2，张秀珍1,2,*

1.山东省海洋水产研究所 2.山东省海洋生态修复重点实验室 3.烟台山水海产有限公司

收稿日期:2012-01-05 修回日期:2012-10-17 出版日期:2012-11-25 发布日期:2012-11-20
通讯作者: 刘慧慧 E-mail:liuhh615@163.com
基金资助:
海洋公益性行业科研专项经费资助项目;新型持久性有机污染物监测与风险评估体系研究示范;基于生态系统的典型海域生物资源综合修复与调控技术研究及示范

Determination of Trifluralin Residues in Aquatic Products by Gas Chromatography

Hui-Hui LIU

Received:2012-01-05 Revised:2012-10-17 Online:2012-11-25 Published:2012-11-20
Contact: Hui-Hui LIU E-mail:liuhh615@163.com

摘要/Abstract

摘要： 建立水产品中氟乐灵残留量的气相色谱检测方法。水产品均质后，用丙酮提取，经正己烷液液萃取，弗罗里硅土固相萃取柱净化后，用气相色谱仪进行测定，外标法定量。该方法在0.5～100ng/mL质量浓度范围内，线性良好，定量限为1.0ng/g。分别在鳗鲡、三疣梭子蟹、文蛤、中国对虾和鲫鱼5种水产品中添加1～10ng/g氟乐灵，回收率在74.8%～99.7%之间。该方法操作简单、灵敏、准确，可以满足水产品中氟乐灵检测要求。

关键词: 气相色谱, 水产品, 氟乐灵

Abstract: A gas chromatography (GC) method was established for determining trifluralin residues in aquatic products in this study. The sample preparation procedure involved homogenization, acetone extraction, n-hexane partition (liquid-liquid extraction) and cleanup on a Florisil solid-phase extraction column before GC analysis. The quantification was performed by external standard method. The GC method showed good linear relationship over the concentration range of 0.5–100 ng/mL. The limit of quantification was 1.0 ng/g. The recovery rates of trifluralin from eel, crab, clams, crucian and shrimp when spiked at 1.0, 2.0 ng/g and 10.0 ng/g were 74.8%–99.7%, respectively. This method was simple, sensitive and accurate, and therefore could meet the requirements for the determination of trifluralin residues in aquatic products.

Key words: gas chromatography (GC), aquatic product, trifluralin

中图分类号:

O657.63

刘慧慧1,2，任传博3，宫向红1,2，徐英江1,2，邓旭修3，张华威3，田秀慧1,2，张秀珍1,2,*. 气相色谱法测定水产品中的氟乐灵[J]. 食品科学, 2012, 33(22): 214-216.

Hui-Hui LIU. Determination of Trifluralin Residues in Aquatic Products by Gas Chromatography[J]. FOOD SCIENCE, 2012, 33(22): 214-216.

参考文献

[1] 朱丽娟，石建忠. 氟乐灵的检验[J]. 刑事技术，2003，1：22-23.
[2] 陈其勇，葛宝坤，韩红芳，等. 粮谷中11种二硝基苯胺类除草剂残留量的气相色谱-串联质谱法测定[J]. 分析测试学报，2011，3（5）：573-576.
[3] 黄灵芝，戴华，李拥军，等. 高效液相色谱法测定荞头中氟乐灵残留量[J]. 食品科学，2004，25(7)：151-153.
[4] 胡敏，李二虎，吴兵兵. 气相色谱法测定大豆中氟乐灵、甲草胺和乙草胺农药残留[J]. 现代农药，2006，5(6)：27-28.
[5] 边照阳，唐纲岭，张洪非，等. 烟草中6种二硝基苯胺类农药残留量的测定[J]. 烟草科技，2010（8），50-54.
[6] 周培，陆贻通，伊雄海. 花生氟乐灵农药残留的优化气相色谱测定法[J]. 上海交通大学学报：农业科学版，2003，21(3)：205-207.
[7] 霍江莲，李军，储晓刚，等. 大豆中二硝基苯胺类除草剂多残留气相色谱法定量检测及质谱确[J]. 分析化学，2006，34(增刊1)：63-67.
[8] 藏小丹，牟光庆. 气相色谱法同时测定大豆中多种除草剂的残留[J].食品研究与开发， 2010，31(3)：132-134.
[9] GARIMELLA U I, SRWARMAN G K, WELLS M J M. Comparison among soil series and extraction methods for the analysis of trifluralin[J].J Agric Food Chem, 2000, 48(12): 5874-5880.
[10] ZHOU Pei, LU Yitong, YI Xionghai, et al. Gas chromatography method for determination of residue trifluralin peanut[J]. Jounral of Shanghai Jiaotong University, 2003, 21(3): 205-207.
[11] MORTIMER R D, BLACK D B, DAWSON B A. Pesticide residue analysis in foods by NMR. 3. comparison of 19F NMR and GC-ECD for analyzing trifluralin residues in field-grown carrots[J]. J Agric Food Chem, 1994, 42(8): 1713-1716.
[12] SMITH A E. Persistence of trifluralin in small field plots as analyzed by a rapid gas chromatographic method[J]. J Agric Food Chem, 1972, 20(4): 829-831.
[13] STRYNAR M, DEC J, BENESI A, et al. Using 19F NMR Spectros-copy to determine trifluralin binding to Soil[J]. Environ sci Technol,2004, 38(24): 6645-6655.
[14] 李孝军，林仙山，王亚楠，等. 超高效液相色谱法测定鳗鱼中氟乐灵残留量[J]. 中国兽医杂志，2011,45（5）：17-19.
[15] 李晓玉，付建，隋涛,等. 气相色谱-质谱联用检测进出口水产品中氟乐灵残留[J].食品科学，2011，32（16）：315-317.