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1 7 Vol. 7 No. 16 Journal of Food Safety and Quality Mar., 16 王 1, 潇 2, 宋维涛 1, 金海燕 1, 丁兰 1* (1., 12; 2., 12) 摘要 : 目的方法,, - (LC-MS/MS) 结果 : 0 W, 0 μl, 1:2, 1 ml; 50 μl, 600 μl, 0.2 g NaCl, μg/kg 62.1%~.1%; 1.6%~6.7% 4.%~. % (n=6), 2 μg/kg 结论, 关键词 : ; - ; ; Rapid extraction of triazine pesticides from tomatoes by microwave-assisted steam diffusion method WANG Xiao 1, 2, SONG Wei-Tao 1, JIN Hai-Yan 1, DING Lan 1* (1. College of Chemistry, Jilin University, Changchun 12, China; 2. Jilin Institute for food Control, Changchun 12, China) ABSTRACT: Objective To extract triazine pesticides in tomato samples by microwave-assisted steam diffusion combined with disperse liquid-liquid microextraction. Methods Tomato samples were extracted by microwave-assisted steam diffusion method, and then obtained extract was purified and enriched by disperse liquid-liquid microextraction. The triazine pesticides were detected using liquid chromatography-tandem mass spectrometry (LC MS/MS) with multiple reactions monitoring (MRM). Results The results of optimized extraction conditions were as follows: microwave forward power was 0 W, the extractant was water vapor with 0 L acetonitrile, the proportion of the sample and quartz sand was 1:2, and the collected volume was 1 ml; and the extractant was 50 L chloroform, the dispersion agent was 600 L acetone, and added 0.2 g NaCl for disperse liquid-liquid microextraction. The recoveries were ranged from 62.1% to.1% for the 6 kinds of triazine pesticides with spiked levels of 1, 50 and 500 μg/kg. The intra- and inter-day relative 基金项目 : (15070GX) Fund: Supported by Development Program of the Ministry of Science and Technology of Jilin Province (15070GX) * 通讯作者 :,, dinglan@jlu.edu.cn *Corresponding author: DING Lan, Professor, College of Chemistry, Jilin University, No. 2699, Qianjin Street, Changchun 12, China. dinglan@jlu.edu.cn

2 7 standard deviation (RSDs) were 1.6%~6.7 % and 4.%~.% (n=6), and the limit of quantitation (LOQ) for the 6 kinds of triazine pesticides was 2 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for triazine pesticides detection in tomato samples. KEY WORDS: triazine pesticides; liquid chromatography-tandem mass spectrometry; tomato; pesticide residues 1 引言, [1] 07 [2],,,, [],, [4-9], Wu [], 92% Rocha [9],, Assadi [],,,, [11-15],,, -,, Biosystems ); ( Eyela );,,.0 mm, 15.0 mm 6, (simazine)(atrazine)(desmetryn) (propazine) (ametryn) (prometryn), Ehrenstorfer, 9% Fisher ; ; Milli-Q 2.2 试验方法溶液配制 : 12.5 mg 6 ml, mg/l, - 6,, 65% mg/l, µg/kg 实验装置和样品萃取过程 1 ; ( ml) ;, 2 材料与方法 2.1 仪器与试剂 NN-GS575WX, 00 W( ); ( ); ABI Q-Trap - ( Applied 1 Fig. 1 Schematic of microwave-assisted steam diffusion combined with disperse liquid-liquid microextraction

KEY WORDS: triazine pesticides; liquid chromatography-tandem mass spectrometry; tomato; pesticide residues 1 引言, [1] 07 [2],,,, [],, [4-9], Wu [], 92% Rocha [9],, Assadi [],,,, [11-15],,, -,,

3 , : 1 (1) 1.0 g ( 0.5 mg/kg),,,, 0 μl, ml, ;,,, (2) (600 L) (50 L),, 500 r/min min, 1 ml, 0 L 2.2. 液相色谱 - 串联质谱条件 (1) ZORBAX SB -C1 (4.6 mm 0 mm, 5 µm), (5:65, V:V), 0. ml/min, ; : μl, : (2) : ESI(+), : 4.5 kv;, : 55 psi; : 50 psi; : medium 0 ; : 1 2, 1 结果与分析.1 微波辅助水蒸气萃取条件优化.1.1 样品与石英砂混合比例 : (1:0 1:4), 2,,,,,,,,,, 1:2 ;,,,,, (1:2, m:m) Table 1 表 1 6 种三嗪类农药的质谱分析参数 MS parameters of 6 kinds of triazine pesticides (m/z) (m/z) (V) (ev) (V) (V) (V) * * * * * * 2 : *

1 微波辅助水蒸气萃取条件优化.1.1 样品与石英砂混合比例 : (1:0 1:4), 2,,,,,,,,,, 1:2 ;,,,,, (1:2, m:m) Table 1 表 1 6 种三嗪类农药的质谱分析参数 MS parameters

4 2 7,, 4,,,,,, 0 W 2 6 (n=6) Fig. 2 Effects of mixed proportion of the sample and quartz sand on recoveries of 6 kinds of triazine pesticides (n=6).1.2 辅助有机溶剂的种类和体积,, (0~500 L),,, 0 L, ;,, 0 L 4 6 (n=6) Fig. 4 Effects of microwave power on recoveries of 6 kinds of triazine pesticides (n=6).1.4 收集萃取液体积, 5 1 ml,,,,, 1 ml 6 (n=6) Fig. Effects of added acetonitrile volume on recoveries of 6 kinds of triazine pesticides (n=6).1. 微波功率, ;,, 5 6 (n=6) Fig. 5 Effects of collection volume on recoveries of 6 kinds of triazine pesticides (n=6)

2 辅助有机溶剂的种类和体积,, (0~500 L),,, 0 L, ;,, 0 L 4 6 (n=6) Fig.

5 , :.2 分散液液微萃取条件优化.2.1 萃取剂的种类和体积, 4,,,, 50 L.2.2 分散剂的种类和体积,,,,,,, L,, 600 L. 方法的线性范围及检出限 5,, µg/kg, 2 (S/N=) (LOD) (LOQ), 6 LOD LOQ 2 5 µg/kg - 7 NaCl 6 (n=6) Fig. 7 Effects of NaCl mass on recoveries of 6 kinds of triazine pesticides (n=6).4 回收率及精密度实验 6 6 (n=6) Fig. 6 Effects of acetone volume on recoveries of 6 kinds of triazine pesticides (n=6).2. 离子强度,,,, 0~0.5 g NaCl, 7 NaCl,, 0.2 g NaCl,,, 0.2 g NaCl, µg/kg : 6, 6 : 1 d, 6 d, 6, %~.1%, 1.6%~6.7% 4.%~.%.5 实际样品测定, 4, 4, 5. µg/kg 4, 5 µg/kg, 67.1%~.4%

7 Effects of NaCl mass on recoveries of 6 kinds of triazine pesticides (n=6).4 回收率及精密度实验 6 6 (n=6) Fig.

6 4 7 5 µg/kg LC-MS/MS Fig. The ion chromatograms of LC-MS/MS with spiked tomato samples (5 µg/kg) 表 2 方法的线性范围, 相关系数, 检出限和定量限 Table 2 Linear ranges, correlation coefficients, LODs and LOQs (µg/kg) (r 2 ) (µg/kg) (µg/kg) 1~00 Y= X ~00 Y= X ~00 Y= X ~00 Y= X ~00 Y= X ~00 Y= X Table 表方法的回收率, 日内和日间精密度 (n=6) Recoveries, RSDs of intra- and inter-day of proposed method (n=6) 1 µg/kg 50 µg/kg 500 µg/kg

(µg/kg) (µg/kg) 1~00 Y=1492.9 + 11.1X 0.999 0.79 2.6 1~00 Y=122.1 + 597.1X 0.995 0.57 1.90 1~00 Y=6014.5 + 66.1X 0.997 0.4 1.62 1~00 Y=5126. + 5.5X 0.997 0.6 2.11 1~00 Y=44.2 + 5.X 0.99 0.54 1.

7 , : 5 4 结论,, -,, 参考文献 [1] Macutkiewicz E, Rompa M, Zygmunt B. Sample preparation and chromatographic analysis of acidic herbicides in soils and sediments [J]. Crit Rev Anal Chem, 0, : [2] Shah J, Jan MR, Ara B, et al. Quantification of triazine herbicides in soil by microwave-assisted extraction and high-performa nce liquid chromatography [J]. Environ Monit Assess, 11, 17: [] Barriuso E, Koskinen WC, Sadowsky MJ. Solvent extraction characterization of bioavailability of atrazine residues in soils [J]. J Agric Food Chem, 04, 52: [4],,, [J]., 16, 5: Wu CY, Bai L, Gu F, et al. Simultaneous determination of 27 triazine herbicides in water using solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry [J]. Environ Chem, 16, 5: [5],,,. - 5 [J]., 15, : Zhang LY, Yao D, Li N, et al. Determination of five triazine herbicides in infant milk powder by high performance liquid chromatography coupled with ionic liquid-based homogeneous liquid-liquid microextraction [J]. Chin J Chromatogr, 15, : [6],,, [J]., 15, 6: Zhang HW, Liu HH, Tian XH, et al. Determination of 9 triazine herbicides in aquatic products by GPC-SPE-GC-MS [J]. J Chin Mass Spectr Soc, 15, 6: [7],,, [J]., 1, 2: Wang XF, Liu XW, Wang L, et al. Determination of twelve triazine herbicide residues in soil by high performance liquid chromatography with accelerated solvent extraction and solid-phase extraction [J]. J Agro-Environ Sci, 1, 2: [] Wu QH, Li Z, Wu CX, et al. Application of ultrasound-assisted emulsification microextraction for the determination of triazine herbicides in soil samples by high performance liquid chromatography [J]. Microchim Acta,, 170: [9] Rocha C, Pappas EA, Huang CH. Determination of trace triazine and chloroacetamide herbicides in tile-fed drainage ditch water using solid-phase microextraction coupled with GC-MS [J]. Environ Pollut, 0, 152: [] Rezaee M, Assadi Y, Hosseinia MRM, et al. Determination of organic compounds in water using dispersive liquid liquid microextraction [J]. J Chromatogr A, 06, 1116: 1 9. [11] Rezaee M, Yamini Y, Faraji M. Evolution of dispersive liquid liquid microextraction method [J]. J Chromatogr A,, 1217: [12] Li Y, Chen PS, Huang SD. Water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction for the determination of organochlorine pesticides in aqueous samples [J]. J Chromatogr A, 1, : [1] Di Napoli-Davis G, Owens JE. Quantitation of tetrabromobisphenol-a from dust sampled on consumer electronics by dispersed liquid-liquid microextraction [J]. Environ Pollut, 1, : [14] Tseng WC, Chu SP, Kong PH. Water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction for the determination of fungicides in wine [J]. J Agric Food Chem, 14, 62: [15] Yuan K, Kang HN, Yue, ZF, et al. Determination of 1 endocrine disrupting chemicals in sediments by gas chromatography-mass spectrometry using subcritical water extraction coupled with dispersed liquid-liquid microextraction and derivatization [J]. Anal Chim Acta, 15, 66: ( 责任编辑 : 金延秋 )

[] Barriuso E, Koskinen WC, Sadowsky MJ. Solvent extraction characterization of bioavailability of atrazine residues in soils [J]. J Agric Food Chem, 04, 52: 6552 6556. [4],,,. - - 27 [J].

8 6 7 作者简介王潇, 工程师, 主要研究方向为食品安全分析 @qq.com 丁兰, 博士生导师, 教授, 主要研究方向为食品和环境安全分析 dinglan@jlu.edu.cn 食药用菌专题征稿函, 00,,,,,,,,,,,, 75%,, 70~0, 50, 12.%, 17.01%,,,,,,,, 16 5,,, 投稿方式 : : jfoodsq@126.com 食品安全质量检测学报编辑部

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0.

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0. 118 217 5 38 1 DOI 1.3969/j.issn.5-6521.217.1.28 Food Research And Development 1 2 1 2 1 2 1 2 1 2 1 2 1. 731 2. 731 - UPLC-MS/MS 5. 1 mol/l ProElut PXC 5 % - Thermo Hypersil Gold mm 2.1 mm 1.9 μm ESI