6 6 Vol. 6 No. 6 2015 6 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., 650223; 2. ( ), 650223) 摘要 : 目的, 方法 -,,, - -0.1%(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 650223, China; 2. Laboratory of Quality & Safety Risk Assessment for Agro-products (Kunming), Ministry of Agriculture, Kunming 650223, 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 (GJFP2015001) Fund: Supported by Risk Assessment of National Agricultural Product Quality in 2015 (GJFP2015001) * 通讯作者 :,, E-mail: 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 650223, China. E-mail: dongshunyang2015@126.com
2284 6 1 引言,, [1], [2-3], 1 1 Fig. 1 The chemical structure of dimethomorph,, ( LD 50 >3900 mg/kg),, [4] (GB 2763-2014) [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 2.2.1 标准溶液配制, 40 μg/ml,, 20 2.2.2 样品处理 25 g 150 ml, 50 ml, 2 min, 6.0 8.0 g NaCl 200 ml, 1 min, 1 h, 1.0 ml 0.22 μm, 2.2.3 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 /% /% 0 95 5 5 10 90 8 10 90 8.1 95 5 10 95 5 2.2.4 质谱条件 [15],, (m/z) 388.2, 301.1 165.2, 66 V, 25 V 45 V
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, -,,, 2 3.2 基质效应的分析 0.1 mg/kg,, - -0.1%(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)
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