Microsoft Word 傅武胜.doc

Size: px

Start display at page:

Download "Microsoft Word 傅武胜.doc"

黯牧
5 years ago
Views:

1 4 1 Vol. 4 No Journal of Food Safety and Quality Feb., 2013 傅武胜 1,2, 郑奎城 1, 邱文倩 1, 王琪林 2, 方勤美 (1.,, ; 2., ; 3., ) 3* 摘要 : 目的 (MG) ; MG, MG, MG, MG 方法 , ; 26 ;, MG LMG 结果 MG 56.1%(37/66), MG (75.8%), MG 0.50~148 μg/kg MG 53.3 ~60.0%, MG 结论 MG, MG, MG, MG MG 关键词 : ; ; ; Investigation and traceability of residual malachite green and its metabolite in freshwater fish FU Wu-Sheng 1,2, ZHENG Kui-Cheng 1, QIU Wen-Qian 1,WANG Qi-Lin 2, FANG Qin-Mei 3* (1. Fujian Provincial Key Laboratory of Zoonosis, Fujian Center for Disease Control and Prevention, Fuzhou , China; 2. Department of Pulic Health, Fujian Medicine University, Fuzhou , China; 3. Biotechnology Research Institute, Fujian Academy of Agricultural Sciences, Fuzhou , China) ABSTRACT: Objective To monitor and assess the residues of malachite green (MG) and its metabolite leuco-malachite green (LMG) in freshwater fish from Fujian and Guangdong provinces. And to carry out the residual traceability of MG for finding the main reasons of high percentage of MG in Chinese perch. Methods A total of 16 kinds of 66 fish samples and 26 water samples were collected from the retailers in Fujian and Guangdong province. After samples being homogenized and pretreated, the concentration of total MG in samples was quantified by high pressure liquid chromatography (HPLC) coupled with fluorescence detector. The MG positive samples analyzed by HPLC were confirmed by HPLC-mass spectrometer (LC-MS/MS). Results The detection rate of MG was 56.1% (37/66) with levels ranged from 0.50 to 148 μg/kg in samples. MG was detected in 75.8% (25/33) of Chinese perch. The detection rate of MG (53.3 ~60.0%) was very similar in freshwater fish sold in Fujian and Guangdong in the retailer. Conclusion High percentage of MG was found 基金项目 : ( ) Fund: Supported by the National Health Welfare Industry-specific Foundation of China ( ) * 通讯作者 :,,, fangqm@126.com *Corresponding author: FANG Qin-Mei, Associate Professor, Biotechnology Research Institute, Fujian Academy of Agricultural Sciences, No.247, Wusi Road, Jinan District, Fuzhou , China. fangqm@126.com

2 1, : 177 in freshwater fish from Fujian and Guangdong province. And no MG was found in water sample from the same cultured pool in the markets. It is indicated that the illegal application of MG in supply chains for Chinese perch may be in the cultivation rather than in the long store and wholesale KEY WORDS: freshwater fish; malachite green; residues; traceability (malachite green, MG) ( 1),, MG, 1933, MG, (LMG) 90, LMG, [1],, MG, , MG, [2] [3] [4] [5] [6] [7] [8], [9] [10] ; MG, MG, MG 6.5%~23.2% [2-8] MG, 2011, MG, MG, MG Fig. 1 1 Chemical structures of malachite green and leuco-malachite green 1 材料与方法 1.1 仪器 LC-20AD ( RF-10AXL, Shimadzu ); Finnigan LCQ deca plus / ( Thermofisher ); DFY-80 ( ); CP225D ( Sartorius ); YP202N ( ); ( IKA ); ( EYELA ); ( Phenomenex ) 1.2 试剂 (Fisher ); (100~200 ), ; PRS (500 mg/3 ml, Varian ) Besep (500 mg/3 ml, ); ( 90.0%), Dr. Ehrenstorfer GmbH MG : MG, 100 μg/ml ; 20 ng/ml MG, 18, LMG ( MG ) 1.3 样品采集与预处理 , 16

3 178 4, 36 ; 30, ~600 g,,, MG 90%,, 26, 50 ml, : 4 12 h,, 4~5, ( r/min),,, CO 2 2 h,, 18, 1.4 MG 的检测方法 (HPLC) [9] : : Symmetry C 18 (250 mm 4.6 mm, 5 μm, Waters ); :35 : - (0.125 mol/l, ph 4.5)(75: 25, v/v); : 1.0 ml/min; (Ex): 265 nm; (Em): 350 nm, LMG, MG LOD 0.5 μg/kg; MG LMG MG, MG 50%~70%, (RSD) 15% 质谱确证 HPLC MG, /, (LMG) m/z 331/ /239, [10] LC-MS/MS, 1.5 质量控制,,, LMG >LOD, 50%~110%, LMG, 2 结果与分析 2.1 养殖鱼 MG 检出的总体状况 2002/675/EC [11], MG LMG 2 μg/kg, MG LMG 40.9%(27/66) MG, (0.5 μg/kg), MG 56.1%(37/66), 2010 (23.2%, 48/207) [6] MG, MG 34.2 µg/kg( 1), 12.2 µg/kg, (10.3 µg/kg),,, 2.2 鱼种间 MG 检出的差异 16, MG 62.5 (10/16), 2010 (53.6%, 15/28) [6] Table 1 表 1 养殖鱼样品中 MG 残留量的分布情况 Distribution of residual malachite green and its metabolite in freshwater fish (µg/kg) < ~1.0 1~2.0 2~10 10~100 > , % % :,

4 1, : 179 (2 ) 6, 7 MG; MG( 2), 3 MG, 3 1 MG; MG (8.33%, 1/12) MG, 2010 (92.6%, 26/28) [6], 75.8%(25/33) 2 MG, 2 1 MG ( 1 ) MG 2.3 桂花鱼 MG 残留的溯源分析,, MG MG 80%, MG,,,, MG 84.6%, ( ) MG ( ) 10 MG 90%, MG,, MG 87.5%, 6 ( ) MG 92.9 (26/28) [6], MG MG, MG( 3), MG MG, MG, MG, MG MG MG MG 表 2 养殖鱼 MG 总量检出情况的对比 Table 2 Comparison of the residual levels of malachite green among some kinds of fish (%) (μg/kg) (μg/kg) (μg/kg) (μg/kg) ~ ~ 表 3 不同环节桂花鱼和养殖水 MG 检出情况的比较 Table 3 Comparison of the detective malachite green in Chinese perch among the selected supply chains MG, MG, μg/kg MG ~ ~ ~ ~ ~ 讨论 3.1 养殖鱼 MG 的总体污染情况 3,, MG 2002 MG, , [12] 66, 37 MG, 56.1%, [2-8] (6.5%~ 23.2%) MG

5 180 4, MG 66, 33, 50%; 2010, 13.5%(28/207) MG, MG 80%, MG 2.38% [6] MG, MG,, ( ) ;, ELISA HPLC LC-MS/MS, HPLC- 17.2%(10/ 58) [6] MG, MG, MG 62.5%, [6] MG (53.5, 15/28) [3] 35.7 (15/42) [8] 57.1%(8/14) MG, MG, MG,,, 3.2 桂花鱼 MG 残留与溯源分析 MG, MG 75.8%, 2010 MG (92.9%) [6], 2006 [13] MG, MG 75.8~90%,, MG, MG, MG,, 2002, MG, MG, MG, MG MG,, MG,,,,,,,,, MG MG, MG MG (80%),, MG 3.3 养殖鱼 MG 残留来源的探讨 MG, MG MG,, MG MG MG MG,,,, MG, MG MG, MG,, MG, MG,, 2006 MG,,, MG MG, MG MG 4 建议 MG, MG, 50%, MG, 4.1 切实从源头上把住安全关

6 1, : 181,,,,, MG 4.2 加强水产品安全的监督监测 MG, MG,, MG,,,, 4.3 加强科研攻关, 提高鱼病防治能力,, MG, MG, 参考文献 [1],,, [J], 2009, 19(3): Li XJ, Tang XZ, Wang SH, et al. Risk assessment of malachite green residue in aquatic product [J]. J Inspect Quarant, 2009, 19(3): [2],,,. [J]., 2006, 16: Ou A, Cai H, Zhuang GR, et al. Investigation report of malachite green residues in breeding shrimp in Zhanjiang area[j] Inspect Quarant Sci, 2006, 16: [3],,,. [J]., 2007, 17(9): Wang LL, Feng CX, Hu EP, et al. Survey of malachite green residues in aquatic foods and pool water from restaurant in Zhuhai [J]. Chin J Health Lab Technol, 2007, 17(9): [4],. [J]., 2008, 14(6): Peng YS, Zhang L. Monitoring and analysis of malachite green in freshwater fish and crabs aquatic products in Ningbo [J]. Strait J Prev Med, 2008, 14(6): [5] [J]., 2010, 20(4): Xiao YH. Monitoring and analysis of malachite green in aquatic foods in Wuhan in 2009 [J]. Chin J Health Lab Technol, 2010, 20(4): [6],,,. [J]., 2011, 23(6): Hua YY, Qiu WQ, Zhou L, et al. Investigation and carcinogenicity risk assessment of freshwater fish malachite green and its metabolite residues in Fujian market [J]. Chin J Food Hyg, 2011, 23(6): [7],,,. [J]., 201l, 22(2): Shao SW, Wen S, Wang Y, et al. Alalysis of malachite green and crystal violet residues in freshwater fishes in Hubei Province [J]. J Public Health Prev Med, 201l, 22(2): [8],,,. [J]., 2012, 29(1): Hu P, Zhao P, Yu SW, et al. Determination of malachite green and crystal violet residues in aquatic products by high performance liquid chromatography [J]. J Shenzhen Univ (Sci Eng), 2012, 29(1): [9], ( ),,. GB/T [S]. :, Chinese Academy of Fishery Sciences, The Ministry of Agriculture Fishery Environment And Aquatic Products Quality Supervision, Inspection And Testing Center (Zhoushan), National Aquatic Products Quality Supervision, Inspection And Test Center, et al. Determination of malachite green and gentian violet residues in fishery products-high performance liquid chromatography with fluorescence detector GB/T [S]. Beijing: China Standards Press, [10]. GB/T [S]. :, Shanghai Entry-Exit Inspection and Quarantine Bureau, China. Determination of malachite green and crystal violet residues in aquatic product GB/T [S]. Beijing: China Standards Press, [11] Commission of the European Communities. Commission Deci-

182 4 sion 2002/675/EC. Implementation Council Directive 96/23/EC n0083658. htm. concerning the performance of analytical methods and the interpretation of results [S].

Teratogenic carcinogenic mutations and the strict inspection of malachite green residues in freshwater fish in China[EB/OL]. [2005-7-15]. http://www.tech-food.

7 182 4 sion 2002/675/EC. Implementation Council Directive 96/23/EC n htm. concerning the performance of analytical methods and the interpretation of results [S] [12], [EB/OL]. [ ]. 7.htm. Teratogenic carcinogenic mutations and the strict inspection of malachite green residues in freshwater fish in China[EB/OL]. [ ]. n htm. [13] [EB/OL].[ ]. Carcinogenic malachite green found in Chinese perch in Hong kong. [ ]. 作者简介 ( 责任编辑 : 张宏梁 ) 傅武胜,,, fwsfqm@126.com 方勤美,, fangqm@126.com

Microsoft Word 聂雪梅.doc

Microsoft Word 聂雪梅.doc 4 4 Vol. 4 No. 4 2013 8 Journal of Food Safety and Quality Aug., 2013 聂雪梅 *, 李立, 孙利, 高飞 (, 100123) 摘要 : 2011 12,, 2007~2011,,,, 关键词 : ; ; ; ; Trade and notification situation on food import and export