PDF《分散液 -液微萃取 -气相色谱法快速检测 番茄中 3 种拟除虫菊...》

2012 年9月Vol.

30 No.

9 September

2012 Chinese Journal of Chromatography

926 ~

930 研究论文 DOI: 10.

3724 / SP. J. 1123. 2012.

06018 ?通讯联系人:陈浩,教授,研究方向为农药残留与食品安全. E-mail: hchenhao@ mail. hzau. edu. cn. 沈菁,副研究员,研究方向为农药残留与食品安全. E-mail: myshengjing@ 126. com. 基金项目:教育部高等学校博士学科点专项科研基金项目(20100146110004). 收稿日期:2012-06-05 分散液-液微萃取-气相色谱法快速检测 番茄中

3 种拟除虫菊酯类农药 李贤波1,2 , 赵1 , 李胜清1 , 陈浩1? , 沈菁2? (1. 华中农业大学理学院, 湖北 武汉 430070;

2. 湖北省农业科学院农业质量标准与检测技术研究所, 湖北 武汉 430064) 摘要:建立了快速(quick)、简单(easy)、便宜(cheap)、有效(effective)、可靠(rugged)和安全(safe)(QuEChERS) 的分散液-液微萃取(DLLME)-气相色谱快速测定番茄中拟除虫菊酯类农药残留的方法. 样品经乙腈提取,N-丙基 乙二胺(PSA)净化,采用 DLLME 富集,用气相色谱法分析. 考察了联苯菊酯、甲氰菊酯和氟氰菊酯在番茄中的残 留测定,同时考察了萃取剂种类与体积、分散剂体积以及萃取时间等因素对萃取效率的影响,以40 μL 氯仿为萃取 剂,1

000 μL 乙腈为分散剂,萃取时间为

60 s. 结果表明:3 种拟除虫菊酯类农药在番茄中的检出限分别为 0.

5、 0.

5、0.

3 μg/ kg. 在

1、10 和50 μg/ kg 添加水平下,联苯菊酯、甲氰菊酯和氟氰菊酯在番茄中的平均回收率分别为 89% ~ 109%、92. 5% ~ 105% 和90% ~ 108%,相对标准偏差分别为 2. 5% ~ 7. 6%、2. 8% ~ 5. 7%、3. 8% ~ 9. 1%. 该方法 简便、快速、安全、价格低廉,重现性好,可用于番茄中拟除虫菊酯类农药的快速检测. 关键词:分散液-液微萃取;

QuEChERS;

气相色谱;

拟除虫菊酯类农药;

番茄 中图分类号:O658 文献标识码:A 文章编号:1000-8713(2012)09-0926-05 Rapid determination of pyrethroids in tomatoes using gas chromatography combined with dispersive liquid-liquid microextraction LI Xianbo1,2 , ZHAO Man1 , LI Shengqing1 , CHEN Hao1? , SHEN Jing2? (1. College of Science, Huazhong Agricultural University, Wuhan 430070, China;

2. Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China) Abstract: An analytical method was established for the determination of three pyrethroids (bifenthrin, fenpropathrin and flucythrinate) in tomatoes using the quick, easy, cheap, effec- tive, rugged and safe ( QuEChERS) cleanup and gas chromatography. The tomato samples were extracted with acetonitrile, cleaned-up by dispersive solid-phase extraction using primary secondary amine as sorbents, concentrated by dispersive liquid-liquid microextraction (DLLME), and analyzed by gas chromatography. Factors affecting the extraction efficiency such as the type and volume of extraction solvent and the volume of dispersive and extraction time were investigated in detail. In the DLLME procedure,

40 μL chloroform was used as the extraction solvent and

1 000 μL acetonitrile was used as the dispersive solvent and the extrac- tion time was

60 s. Under the optimized conditions, the limits of detection for bifenthrin, fen- propathrin and flucythrinate were 0. 5, 0.

5 and 0.

3 μg / kg, and the average recoveries in toma- to samples at the spiked levels of 1,

10 and

50 μg / kg were 89% - 109%, 92. 5% - 105% and 90% - 108% with the relative standard deviations of 2. 5% - 7. 6%, 2. 8% - 5. 7% and 3. 8% - 9. 1%, respectively. The proposed method is simple, quick, safe, reliable and applicable to analyze 第9期李贤波,等:分散液-液微萃取-气相色谱法快速检测番茄中