Microsoft Word _排版二校

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渔球驾钮祜禄
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1 8 2 Vol. 8 No Journal of Food Safety and Quality Feb., 2017 李佳蔚, 黄 * 会, 韩典峰, 罗晶晶, 薛敬林, 邹荣婕, 刘慧慧, 宫向红 (,, ) 摘要 :,,,,, C 18,, -,, 关键词 : ; ; Research progress of the toxicity and multi-residue detection technology of sulfonylurea herbicides LI Jia-Wei, HUANG Hui, HAN Dian-Feng, LUO Jing-Jing, XUE Jing-Lin, ZOU Rong-Jie, LIU Hui-Hui, GONG Xiang-Hong * (Shandong Provincial Key Laboratory of Restoration for Marine Ecology, Shandong Marine Resource and Environment Research Institute, Yantai , China) ABSTRACT: Sulfonylurea herbicides are highly effective, broad-spectrum, highly selective herbicides for controlling broadleaf weeds and gramineous weeds. Sulfonylurea herbicides play an important role in modern agricultural production, but their pesticide residues also have many negative effects on the ecological environment and safety of agricultural products. This paper mainly reviewed toxic hazards of sulfonylurea herbicides, limits of standards, pre-treatment of residual detection and instrumental analysis methods. At present, the detection of sulfonylurea herbicide residues mainly involve soil and water, as well as grain, animal-derived food and other matrixes. The domestic pre-treatment method commonly used for the detection of such herbicide residues is solid phase extraction method and C 18 is the common filler. Liquid chromatography-mass spectrometry has become the preferred method for such herbicide analysis due to its high sensitivity and the ability that can detect trace levels of residues. At the same time, the residual detection of herbicides has been developed from single residue detection to 基金项目 : (SDAIT-12-09) (SDAIT-14-08) (SDAIT-26-05) ( ) ( NC-1). Fund: Supported by Shandong Province Modern Agricultural Technology System Fish Industry Innovation Team (SDAIT-12-09), Shandong Province Modern Agricultural Technology System Shellfish Industry Innovation Team(SDAIT-14-08) and Shandong Province Modern Agricultural Technology System Algae Industrial Innovation Team(SDAIT-26-05); Special Fund for Agro-scientific Research in the Public Interest( NC-1). * 通讯作者 :,,. ggxxhh123@163.com *Corresponding author: GONG Xiang-Hong, Professor, Marine Fisheries Research Institute of Shandong Province, No.216, Changjiang Road, Yantai , China. ggxxhh123@163.com

2 368 8 multi-residue detection. KEY WORDS: sulfonylurea herbicides; toxicity; multi-residue detection technology 1 引言,,, (chlorsulfuron),, [1], 2% [2], 40, (nicosulfuron) (metsulfuron-methyl) (thifensulfuron- methyl) (triasulfuron) (bensulfuron) (chlorimuron-ethyl) (pyrazosulfuron-ethyl) [3], [1], 10%~30% [5],,,,,,,, , , [4], 2 磺酰脲类除草剂毒性与危害, 2.1 对植物的毒性 (ethametsulfuron-methyl),,,, [5-7],, 1 μg/kg,, 10 μg/kg [8], 3~5, 2.2 对水生生物的毒性,,, [9], ( ),,,, [10,11], [12], (tribenuron-methyl), ; [13],, ;, (20 mg/l 40 mg/l), [14] [15], ; Miron [16],,, Wendt-Rasch [17] Cedergreen [18], [19] (halosulfuron-methyl) 96 h (LC 50 ) 21.7 mg/l, 5% -21% 96 h LC mg a.i./l; 溞 48 h EC mg a.i./l, [20], ATP ;,,, ATP AchE, [21], 15.2 d,

3 2, : h mg/l [22] 3 磺酰脲类除草剂相关限量标准 (maximum residue limit, MRL) 0.05 mg/kg, MRL 0.02 mg/kg [23] GB , MRL 0.05 mg/kg, MRL 0.1 mg/kg, MRL 0.1 mg/kg, MRL 0.05 mg/kg [24] MRL mg/kg [25] 2006 MRL 0.02 mg/kg [25] 4 磺酰脲类除草剂残留检测方法 [26] [27] [28] [29] 4.1 前处理方法, C 18 (hydrophile-lipophile balance, HLB) (florida silica, FLO) (molecularly imprinted polymer, MIPs) (multiwalled carbon nanotube, MWCNTs) HLB N-, [30] [31], -, HLB, - (high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS),,, 0.3 mg/kg [29], HLB, 20 C 18,,,, [32], C 18,, 10 μg/l, 81.6%~90.9% [33] 3,, C 18 - (ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS), 0.12~0.16 μg/kg, 81.4%~92.9%, 5.5%~10.6% [34], C 18, 3 3, [35] QuEChERS - (liquid chromatography-tandem mass spectrometry, LC-MS/MS) 32, Z-Sep/C 18, ~5.0 μg/kg [26] Oasis HLB C 18, 3 SPE,, C 18,,, LC-MS/MS 6,,, 1.0 ng/ml, 84.2%~95.0%, [36] (molecular imprinting technique, MIT),,,,,, 4, [37], 0.1%, 7 (magnetic solid-phase extraction, MSPE), SPE,,,, [38] -, 5 [39] 6, 6, 0.019~0.037 μg/l, 92.6%~105.7% 89.8%~108.7%, 0.7%~7.1% 0.5%~4.0% 1

4 370 8 Table 1 表 1 磺酰脲类除草剂残留检测的前处理方法 Pretreatment methods for sulfonylurea herbicides residues (μg/l, μg /kg) [26] C ~0.16 [33] 10 HLB 0.6~3.5 [31] 13 HLB 0.020~0.092 [30] ~0.47 [36] ~0.2 [37] 16 SPE 0.2~0.8 [40] 5 /Fe3O ~0.04 [38] 6 C ~0.037 [39] 12 RP [41] 12 Bond Elut-PPL 0.003~0.16 [42] 10 C ~0.04 [43] 5 C ~0.70 [44] 7 HLB 0.32~0.62 [45] 12 C ~20 [34] [25] 32 C ~5. 0 [35] 20 HLB [29] 4.2 仪器分析方法 (high performance liquid chromatography, HPLC) - (liquid chromatography-tandem mass spectrometry, LC-MS/MS), (capillary electrophoresis, CE) (fluorescence analysis, PCF), (gas chromatographic, GC),,, 高效液相色谱法及液相色谱 - 质谱联用法 HPLC,,,, LC-MS/MS,, [46] 3 (reversed phase high performance liquid chromatography, RP-HPLC) C 18 ; C 18 - (RP-HPLC-DAD) 3 0.1~10.0 mg/l, ~ %~98.3% 80.2%~107.6%, 1.39%~7.82%, [32] UPLC-MS/MS C 18 ;, UPLC-MS/MS 0.01~1 mg/l, %~90.9% 107.9%~111.5% 99.0%~105.2%, 1.7%~15.7%, 10 μg/kg [28], 10 RP-HPLC, - Florisil, RP-HPLC-DAD, 20 μg/kg 毛细管电泳法 CE,

5 2, : 371,,, [47] 3,, 1.0~10 mg/l, 82%~109%, 3%(n=6), 30~50 μg/kg 荧光分析法,, [48] 0~151 μg/l, r , 0.8 μg/l 2 5 结论与展望,,,,, C 18,,,,,, Table 2 表 2 磺酰脲类除草剂残留的检测方法回收率检出限及相对标准偏差 Detection methods, recoveries, detection limits and relative standard deviations of sulfonylurea herbicides residues /% /(μg/l) RSD/% 4 HPLC 89.3~ ~ ~5.79 [36] 6 LC-MS/ MS 84.2~ ~6.70 [26] 10 HPLC-MS 80.2~ ~ ~4.26 [31] 13 HPLC-MS/MS 89.0~ ~ ~11.2 [30] 3 UPLC-MS/MS 81.4~ ~ ~10.6 [33] 3 RP-HPLC-DAD 80.2~ ~7.82 [46] 3 CE 82.0~ ~50.0 <3.00 [47] 7 LC-ESI-MS/MS 81.5~ ~0.20 ng/l 0.30~7.00 [37] 12 LC-DAD 84.0~ ~0.16 [42] 5 HPLC 72.8~ ~ ~4.10 [49] 5 HPLC-UV 73.0~ ~ ~4.15 [44] 12 HPLC-DAD 7.01~ ~14.0 [41] 3 RP-HPLC-DAD 80.2~ ~7.82 [48] 16 UPLC-MS/MS 72.1~ ~ ~8.90 [40] UPLC-MS/MS 81.6~ ~8.90 [32] 11 UPLC-MS/MS 85.6~ ~ ~9.40 [50] 12 HPLC 72.2~ ~ ~6.40 [34] 10 RP-HPLC-DAD 69.8~ ~10.4 [25] 32 LC-MS/MS 80.0~ ~ ~13.0 [35] 20 HPLC-MS/MS 66.1~ ~19.4 [29]

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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

Microsoft Word _排版 二校

Microsoft Word _排版二校