Microsoft Word 林涛-二校回出2283、2287

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1 6 6 Vol. 6 No Journal of Food Safety and Quality Jun., 2015 林 1, 涛 2, 樊建麟 1, 黎其万 1, 李彦刚 1, 杨东顺 1* (1., ; 2. ( ), ) 摘要 : 目的, 方法 -,,, %(V:V) -1 mmol/l 3 结果,, -0.1%(V:V), 结论, 关键词 : ; ; ; Study on the matrix effects of dimethomorph in fruits and vegetables LIN Tao 1, 2, FAN Jian-Lin 1, LI Qi-Wan 1, LI Yan-Gang 1, YANG Dong-Shun 1* (1. Institute of Agriculture Quality Standards & Testing Technique, Yunnan Academy of Agricultural Science, Kunming , China; 2. Laboratory of Quality & Safety Risk Assessment for Agro-products (Kunming), Ministry of Agriculture, Kunming , China) ABSTRACT: Objective To increase the accuracy of dimethomorph detection in orange and celery by studying the matrix effect. Methods The detection were conducted on an ultra performance liquid chromatography-tandem mass spectrometry, the effect of 3 kinds of mobile phases including methanol-water, methanol-0.1% (V:V) formic acid solution and methanol-1 mmol/l ammonium acetate solution on the matrix effects were compared. Dimethomorph in orange and celery samples was extracted by acetonitrile. Positive ion mode and multiple reaction monitoring were used in the analysis and external standard method was used for quantification. Also, the effect of preparation methods of standard solutions including diluted with methanol and blank matrix were studied. Results The matrix effects of dimethomorph were effectively inhibited when the standard solution was diluted with blank matrix, and the matrix effects of dimethomorph were partly inhibited when the mobile phase was methanol-0.1%(v:v) formic acid solution in determination of dimethomorph in oranges and celery. Conclusions This method is simple and fast, which can provide a reference for the study of matrix effects of dimethomorph in other fruits and vegetables. KEY WORDS: orange; celery; dimethomorph; matrix effect 基金项目 : 2015 (GJFP ) Fund: Supported by Risk Assessment of National Agricultural Product Quality in 2015 (GJFP ) * 通讯作者 :,, dongshunyang2015@126.com *Corresponding author: YANG Dong-Shun, Associate Researcher, Institute of Agriculture Quality Standards & Testing Technique, Yunnan Academy of Agricultural Science, No. 9, Xueyun Road, Wuhua District, Kunming , China. dongshunyang2015@126.com

2 引言,, [1], [2-3], 1 1 Fig. 1 The chemical structure of dimethomorph,, ( LD 50 >3900 mg/kg),, [4] (GB ) [5], 0.5 mg/kg, [6] [7] - [8,9] - [10,11],, [12], [13,14],,,,, -,, 2 材料与方法 2.1 仪器与试剂 API4000 ( AB ); 1290 ( Agilent ); ZORBAX RRHD 2.1 mm 50 mm, 1.8 µm ( Agilent ); T18 ULTRA-TURRAX ( IKA ); AE100 ( METTLER TOLEDO ) (, Merck ); (, Merck ); ( ); (1000 mg/l, ); ( ) 2.2 实验方法 标准溶液配制, 40 μg/ml,, 样品处理 25 g 150 ml, 50 ml, 2 min, g NaCl 200 ml, 1 min, 1 h, 1.0 ml 0.22 μm, 色谱条件, 1, : 35 ; : 0.2 ml/min; : 1 μl 表 1 梯度洗脱参数 Table 1 Gradient elution parameters /min /% /% 质谱条件 [15],, (m/z) 388.2, , 66 V, 25 V 45 V

3 6, : 2285 Fig. 2 2 The chromatogram of dimethomorph 3 结果与分析 3.1 仪器条件的优化,,,, 2, -,,, 基质效应的分析 0.1 mg/kg,, %(V:V) -1 mmol/l, 3, -,, ; -0.1%(V:V) -1 mmol/l, 80%, 3 ( ) Fig. 3 The matrix effects in orange and celery with different mobile phases (The standard solution was diluted with methanol)

4 2286 6,, 3,, 4, ; -1 mmol/l, 4 ( ) Fig. 4 The matrix effects in orange and celery with different mobile phases (The standard solution was diluted with blank matrix) 4 结论与讨论,,, [13],, -,,,,,,,,,,,,, 参考文献 [1],,,. [J]., 2011, 50(1): Wang Y, Yao WF, Liang S, et al. Residues determination of pyraclostrobin dimethomorph in cabbage and soil [J]. Pesticides, 2011, 50(1): [2] Kuhn PJ, Pitt D, Lee SA, et al. Effects of dimethomorph on the morphology and ultrastructure of phytophthora [J]. Mycological Res, 1991, 95(3): [3] Cohen Y, Baider A, Cohen BH. Dimethomorph activity against oomycete fungal plant pathogens [J]. Phytopathology, 1995, 85(12): [4] Rekanović E, Potočnik I, Milijašević-Marčić S, et al. Toxicity of metalaxyl, azoxystrobin, dimethomorph, cymoxanil, zoxamide and mancozeb to Phytophthora infestans isolates from Serbia [J]. J Environ Sci Health, Part B, 2012, 47(5): [5] GB [S]. GB National food safety standard-maximum residue limits for pesticides in food[s]. [6],,,. [J]., 2011, 13(2): Pu XY, Tao CJ, Jiang H, et al. Study on degradation dynamics of Z-and E-isomers of dimethomorph in soils [J]. Chin J Pestic Sci, 2011, 13(2): [7] Liang H, Li L, Li W, et al. Dissipation and residue of dimethomorph in pepper and soil under field conditions[j]. Ecotoxicol Environ Saf, 2011, 74(5): [8] Sannino A, Bolzoni L, Bandini M. Application of liquid chromatography with electrospray tandem mass spectrometry to the determination of a new generation of pesticides in processed fruits and vegetables [J]. J Chromatogr A, 2004, 1036(2): [9] Kujawski MW, Bargańska Ż, Marciniak K, et al. Determining pesticide contamination in honey by LC-ESI-MS/MScomparison of pesticide recoveries of two liquid liquid extraction based approaches [J]. LWT- Food Sci Technol, 2014, 56(2): [10] Hengel MJ, Shibamoto T. Gas chromatographic-mass spectrometric method for the analysis of dimethomorph fungicide in dried hops [J]. J Agric Food Chem, 2000, 48(12): [11] Páleníková A, Martínez-Domínguez G, Arrebola FJ, et al.

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