8 1 Vol. 8 No. 1 2017 1 Journal of Food Safety and Quality Jan., 2017 2013~2015 闻 胜 1, 熊碧 1, 黄常刚 2, 梁高道 2, 何振宇 2, 刘潇 1, 张瑞陈明 1 1*, 宋毅 (1.,, 430079; 2., 430015) 1, 摘要 : 目的 2013~2015, 方法 (furaltadone) (nitrofurazone) (nitrofurantoin) (furazolidone)4, Excel SPSS 16.0 结果 27.09%, (semi carbazide, SEM),, 61.54%; 6.78%; 1.38%;, 91.67%; SEM 结论, SEM, SEM 关键词 : ; ; ; Monitoring and analysis of nitrofuran metabolites residues in shrimp of Hubei area in 2013~2015 WEN Sheng 1, XIONG Bi 1, HUANG Chang-Gang 2, LIANG Gao-Dao 2, HE Zhen-Yu 2, LIU Xiao 1, ZHANG Rui 1, CHEN Ming 1, SONG Yi 1* (1. Hubei Provincial Key Laboratory for Applied Toxicology, Hubei Provincial Centre for Disease Control and Prevention, Wuhan 430079, China; 2. Wuhan Centre for Disease Control and Prevention, Wuhan 430015, China) ABSTRACT: Objective To analyze the nitrofuran metabolites residues in shrimp of Hubei area in 2013~2015, so as to provide scientific basis for the source and hazard analysis. Methods The residues of 4 kinds of nitrofuran metabolites including furaltadone, nitrofurazone, nitrofurantoin and furazolidone in shrimp of Hubei area were detected by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and the obtained data were statistically analyzed by Excel and SPSS16.0. Results The detection rate of nitrofuran metabolites was 27.09%, and all of them were semi carbazide (SEM), while river prawn had the highest detection rate of 61.54%, followed by shrimps of 6.78% and crawfish of 1.38%. For overall homogenate river shrimp, the detection rate was up to 91.67%, while SEM was not detected in the shelled shrimp samples. Conclusion Different levels of SEM are 基金项目 : (WJ2016J-023) Fund: Supported by the Health and Family Planning Commission of Hubei Provincial Project (WJ2016J-023) * 通讯作者 :,, E-mail: 16062518@qq.com *Corresponding author: SONG Yi, Associate Chief Technician, Hubei Provincial Key Laboratory for Applied Toxicology, Hubei Provincial Centre for Disease Control and Prevention, Wuhan 430079, China. E-mail: 16062518@qq.com
1, : 2013~2015 337 detected in shrimp of Hubei area, meanwhile endogenous SEM is founded in river prawn. According to the food consumption data of residents in Hubei area, the SEM exposure in shrimp is less harmful to human health. KEY WORDS: shrimp; nitrofuran; metabolite; residue monitoring 1 前言 5-,, A,, [1,2] 4, (furaltadone) (nitrofurazone) (nitrofurantoin) (furazolidone) [3], [4-7] [5-7] ; 2015,, 1 μg/kg [8] 2002, ( 193 ) [9] ; 2005 ( 560 ), [10] ( ) ( 2010 50 ), [11], DNA, : 3- -5- -2- (5-morpholine-methyl-3- amino-2-oxazolidinone, AMOZ) (semi carbazide, SEM) 1- (1-aminohydantoin, AHD) 3- -2- (3-amino-2-oxazolidinone, AOZ) 2015, 455, 5.2%, 20 [12] ( :, Procambarus clarkii), 70% [13] (, :, Macrobrachium nipponense) ( :, Metapwnaeus ensis),,, 2 材料和方法 2.1 材料 2.1.1 仪器 UPLC-TQD ( Waters ); PRO200 ( PRO ); Z383K ( Hermle ); SHZ-88 ( 37±1, ); Vortex-Genie 2 ( Scientific Industries ); N-EVAPTM112 ( Organomation Associates ) 2.1.2 试剂 AOZ(50 mg, 99.7%) AMOZ(10 mg, 100%) SEM(50 mg, 99.5%) AHD(50 mg, 99.3%) D4-AOZ(10 mg, 100%) D5-AMOZ(10 mg, 100%) 13 C 15 N-SEM(10 mg, 100%) 13 C-AHD(10 mg, 100%), WiTEGA Laboratorien Berlin-Adlershof GmbH ; (, TEDIA ); ( TCI ); Oasis HLB ( Waters ); (, ); 2.2 实验方法 2.2.1 样品采集, 2013~2015, 9 ( ) 347 : 145 143 59, 2.2.2 样品制备,,,, 2013 2014, 500 g, -20 2.2.3 样品分析 - [14] 1 g( 0.01 g), 50 ml, 100 μl 100.0 ng/ml 200 μl 0.1 mol/l 10 ml 0.2 mol/l, 37 16 h
338 8, ph 7~8, 4 10000 r/min 10 min, Oasis HLB, 5 ml, 5 ml,, 1.0 ml (50:90, V:V), 0.45 µm 2.2.4 数据分析 Excel 2007, Excel SPSS 16.0 86.67%, 2014 93.94%( 1) 2013 SEM 2014, 2 (Χ 2 1.428, P 0.232) 2015 SEM SEM, SEM, SEM 3 结果与讨论 3.1 虾产品中硝基呋喃类代谢物监测总体状况 2013~2015, 9 347, 27.09%,, 61.54%;, 6.78%;, 1.38% ( ), 91.67%( 1) 1, 2013~2015, SEM, 100% 2.3~246 μg/kg; 3 (AMOZ AOZ AHD), 246 μg/kg, 2.8 μg/kg, 2, 78.1 2.3 μg/kg,, 3.2 不同年份虾产品中硝基呋喃类代谢物监测状况分析 2013 SEM 1.47%, 2014 2015 SEM, 91.67%, 2013 1 2013~2015 Fig. 1 Detection situation of nitrofurans metabolites in shrimp from Hubei area in 2013~2015 3.3 SEM 来源分析 SEM,, SEM,, SEM, SEM SEM, : SEM, SEM ; SEM,,, SEM, SEM [15] ;, Table 1 表 1 湖北地区虾产品中硝基呋喃类药物检出情况 Determination of nitrofurans metabolites residues in shrimp from Hubei area (%) SEM (μg/kg) AOZ SEM AMOZ AHD ( ) 145 2 1.38 0 2 0 0 2.3~78.1 / / / 143 88 61.54 0 88 0 0 2.8~246 85.0 45.0 77.2 96 88 91.67 0 88 0 0 2.8~246 85.0 45.0 77.2 47 0 0 0 0 0 0 / / / / ( ) 59 4 6.78 0 4 0 0 9.9~95.6 35.1 40.8 17.4 347 94 27.09 0 94 0 0
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