Microsoft Word 陈永平-----参考文献标号错误.doc

4 1 Vol. 4 No. 1 2013 2 Journal of Food Safety and Quality Feb., 2013 陈 永 平 *, 张 素 青, 李 春 青, 李 连 庆, 马 丹, 高 丽 娜, 张 萍 (, 300221) 摘 要 : 目 的 方 法, HPLC, SPSS 结 果 10 50 100 µg/kg, 57.9% 48.0% 23.0%, 46.6% 43.4% 19.8% 50 µg/kg, K (50 µg/kg) =0.00338 d 1, K (50 µg/kg) =0.00268 d -1, K( 50 µg/kg )=0.00359 d 1, K (50 µg/kg) =0.00321 d 1 K (111.2 µg/kg, )=0.000614 d 1, K (50 µg/kg, )=0.00125 d 1 结 论 ; ; 关 键 词 : ; ; ; Studies on degradation kinetics of malachite green and leucomalachite green in different aquatic products CHEN Yong-Ping *, ZHANG Su-Qing, LI Chun-Qing, LI Lian-Qing, MA Dan, GAO Li-Na, ZHANG Ping (Superision and Test Center for Fisheries Environment and Quality of Fishery Products of Ministry Agriculture, Tianjin 300221, China) ABSTRACT: Objective To study degradation kinetics of malachite green and leucomalachite green in different aquatic products. Methods After extracted and purified, samples were detected by high pressure liquid chromatography, and the results were analyzed with SPSS software and degradation kinetics software. Results Degradation of malachite green and leucomalachite green in different aquatic products matrix was fit to pseudo-first order kinetics equations.the degradation rates of malachite green were 57.9%, 48.0%, 23.0%, and the degradation rates of leucomalachite green were 46.6%, 43.4%, 19.8% in three aquatic products matrixes, respectively. For carp matrix added concentration of 50 µg/kg, malachite green and leucomalachite green degradation rate constants were K (50 µg/kg) =0.00338 d 1, K (50 µg/kg)=0.00268 d 1 in natural thawing.and K (50 µg/kg) = 0.00359 d 1, K (50 µg/kg) =0.00321 d 1 in microwave thawing, respectively. The leucomalachite green degradation rate constants in practical samples were K (111.2 µg/kg carp ) =0.000614 d 1, and K (50 µg/kg carp ) =0.00125 d 1. Conclusion Degradation rates of malachite green was faster than that of leucomalachite green. Compared with higher * 通 讯 作 者 :,, E-mail: yongping008@yahoo.com.cn *Corresponding author: CHEN Yong-Ping, Engineer, Superision and Test Center for Fisheries Environment and Quality of Fishery Products of Ministry Agriculture, NO. 442, Jiefangnan Road, Hexi District, Tianjin 300221, China. E-mail:yongping008@yahoo.com.cn

184 4 concentration, the degradation in low concentration was faster. Two kinds of ways of thawing had no effects on the degradation of malachite green and leucomalachite green. The leucomalachite green degradation rate in practical samples was slower than that in the blank matrix added of leucomalachite. KEY WORDS: malachite green; leucomalachite green; aquatic products; degradation kinetics 1 引 言,,,,, [1-2],, [3-6],, [7] [8],,,,, 2 材 料 与 方 法 2.1 材 料 与 仪 器 :,, ; :, ; Sigma : Agilent 1200( ); (0.0001 g) (0.001 g) - ; (, 10000 r/min); ( Sigma, 10000 r/min); ( ); : 1.0 mg( 0.01 mg) ( ), 10.0 ml, 100 µg/ml (1.0 μg/ml): ( ) 1.0 ml, 100 ml, 18 3 2.2 实 验 样 品 的 制 备 及 分 组 (5±0.02)g 50 ml ( 150, 90 ), 10.0 50.0 100.0 μg/kg, (1 2 4 10 20 40 60 90 120 150 180 210 d), 50 μg/kg 2.3 分 析 方 法 5.00 g, 1,, 2,, 6000 r/min,, 40 ml,, 50 ml,, 3 ml, 1 ml, SPSS 2.4 测 定 : Agilent XDB-C 18, 5 µm, 4.6 mm 150 mm; ; : 50 µl; : 1.2 ml/min; VWD : 588 nm : ( ph 4.5): =20 80(v/v) 3 结 果 与 分 析 2.4 100 ng/ml 50 µg/kg,,

1, : 185 1 100 ng/ml (100 ng/ml) Fig. 1 Chromatogram of MG and LMG (100 ng/ml) 2 50 µg/kg Fig. 2 Chromatogram of MG in carp sample (50 µg/kg),, 100 ng/ml 1 2 1 2 3 10 50 100 µg/kg 1 2 4 10 20 40 60 90 120 150 180 210 d,, 10 µg/kg, 50 µg/kg, 100 µg/kg,, SPSS, F, α<0.01 X t/d, Y t Ct, K 10 50 100 µg/kg, : K (10 µg/kg, )=0.005770 d 1, K (10 µg/kg, )=0.00315 d 1, K (10 µg/kg, )=0.004076 d 1 ; K (50 µg/kg, )= 0.00338 d 1, K (50 µg/kg, )=0.00264d 1, K (50 µg/kg, )= 0.00334 d 1 ; K (100 µg/kg, )=0.00145 d 1, K (100 µg/kg, )= 0.00127 d 1, K (100 µg/kg, )=0.00128 d 1 ; : K (10 µg/kg, )=0.00425 d 1, K (10 µg/kg, )=0.00338 d 1,

186 4 表 1 鲤 鱼 组 织 中 有 ( 无 ) 色 孔 雀 石 绿 降 解 浓 度 - 时 间 表 Table 1 Concentration-time of MG and LMG in carp matrix (µg/kg) /d 10 50 100 MG/LMG LMG MG/LMG LMG MG/LMG LMG 1 9.4 9.6 42.4 45.1 93.3 94.5 2 9.1 9.4 41.6 44.5 92.6 94.0 4 8.8 9.2 39.8 43.3 91.2 93.1 10 8.4 8.9 38.5 41.2 89.4 92.3 20 7.7 8.6 36.2 39.1 88.5 90.4 40 6.9 8.2 34.4 37.2 86.7 88.6 60 6.1 7.6 31.3 35.5 84.1 87.2 90 5.3 7.0 29.1 33.6 81.5 84.7 120 4.5 6.5 27.3 31.4 78.1 81.3 150 3.8 5.9 24.5 29.6 76.4 78.5 180 3.3 5.3 22.8 27.6 72.2 76.6 210 3.0 4.8 20.5 24.5 70.7 74.3 表 2 鳗 鲡 组 织 中 有 ( 无 ) 色 孔 雀 石 绿 在 降 解 浓 度 - 时 间 表 Table 2 Concentration-time relationship of MG and LMG in eel matrix (µg/kg) /d 10 50 100 MG/LMG LMG MG/LMG LMG MG/LMG LMG 1 9.2 9.4 41.1 43.4 92.6 93.7 2 9.1 9.3 40.5 42.6 91.8 93.5 4 8.9 9.1 39.4 41.4 90.4 93.1 10 8.6 8.9 38.2 40.1 88.7 92.4 20 8.2 8.6 36.8 38.5 87.7 91.5 40 7.7 8.3 35.1 37.5 86.1 89.7 60 7.2 7.9 33.3 35.3 84.4 87.9 90 6.6 7.4 32.6 33.4 82.5 85.6 120 6.2 6.8 30.4 31.1 80.2 83.4 150 5.8 6.4 28.4 29.7 77.7 82.1 180 5.5 5.9 26.5 28.1 74.5 80.4 210 4.9 5.4 24.2 26.5 73.8 78.5 表 3 鳜 鱼 组 织 中 有 ( 无 ) 色 孔 雀 石 绿 降 解 浓 度 - 时 间 表 Table 3 Concentration-time of MG and LMG in mandarinfish matrix (µg/kg) /d 10 50 100 MG/LMG LMG MG/LMG LMG MG/LMG LMG 1 9.3 8.9 42.3 45.2 94.3 94.4 2 9.1 8.8 41.2 44.3 93.6 93.7 4 8.7 8.6 40.3 43.6 92.2 92.8 10 8.2 8.3 38.4 41.9 90.9 91.1 20 7.8 7.9 36.1 40.5 88.8 89.5 40 7.3 7.7 34.5 38.2 86.4 87.3 60 6.5 7.3 32.6 36.1 84.8 85.6 90 5.7 6.8 29.7 33.9 81.7 83.5 120 5.1 6.5 27.2 31.5 78.1 81.2 150 4.7 5.9 24.4 29.4 76.7 79.6 180 4.4 5.3 22.8 27.3 74.4 76.5 210 3.8 4.7 20.7 24.6 71.3 73.7

1, : 187 K (10 µg/kg, )=0.00387 d 1 ; K (50 µg/kg, )=0.00268 d 1, K (50 µg/kg, )=0.00145 d 1, K (50 µg/kg, )=0.00275 d 1 ; K (100 µg/kg, )=0.00127 d 1, K (100 µg/kg, )=0.00085 d 1, K (100 µg/kg, )=0.00110 d 1,, Table 4 表 4 鲤 鱼 组 织 不 同 解 冻 方 式 及 阳 性 样 品 中 有 ( 无 ) 色 孔 雀 石 绿 降 解 浓 度 - 时 间 表 Concentration-time of MG(LMG) by different thawing mode and positive samples in carp matrix (50 µg/kg) t/d Sample 1 Sample 2 MG/LMG LMG MG/LMG LMG LMG LMG 1 42.4 45.1 41.0 44.4 111.2 54.6 2 41.6 44.5 40.2 43.5 110.5 54.3 4 39.8 43.3 39.3 42.7 109.6 53.9 10 38.5 41.2 38.5 41.8 108.8 53.2 20 36.2 39.1 37.2 40.4 107.7 51.6 40 34.4 37.2 35.6 38.9 106.5 50.3 60 31.3 35.5 32.8 36.2 104.8 48.8 90 29.1 33.6 29.5 33.1 103.3 47.2 120 27.3 31.4 26.4 30.5 102.2 45.6 150 24.5 29.6 23.6 27.3 101.3 44.4 180 22.8 27.6 21.3 24.6 99.6 43.2 210 20.5 24.5 18.5 21.2 95.4 42.4 Table 5 µg/kg 表 5 鲤 鱼 鳗 鲡 鳜 鱼 组 织 中 不 同 浓 度 有 无 色 孔 雀 石 绿 210 d 后 降 解 率 表 Degradation rate of different MG(LMG) spiked concentration in carp, eel and mandarinfish matrix after 210 d MG/LMG LMG MG/LMG LMG MG/LMG % LMG 1/LMG 2/LMG 10 68 50 46.7 42.5 59.1 47.2 --- --- 50 51.7 45.7 41.1 38.9 51.1 45.6 --- --- 100 24.2 21.4 20.3 16.2 24.4 21.9 --- --- 114.2 --- --- --- --- --- --- 14.2 --- 54.6 --- --- --- --- --- --- --- 12.2 4,,, y=c t /C 0, 5 10 50 100 µg/kg 57.9% 48.0% 23.0%, 46.6% 43.4% 19.8%, 50 µg/kg K (50 µg/kg, )=0.00338 d 1, K (50 µg/kg, )=0.00268 d 1, K (50 µg/kg, )= 0.00359 d 1, K (50 µg/kg, )=0.00321 d -1,,, K (111.2 µg/kg, )= 0.000614 d 1, K (50 µg/kg, )=0.00125 d 1,,,

188 4 4 结 论,, : 10 50 100 µg/kg, 50 µg/kg,, spss,,,,,, 参 考 文 献 [1],,. [J]., 2007, 22(4): 294 298. Gui YA, Wang HJ, Liu CL. Potential hazards of malachite green residues and itsmetabolites and detection in aquatic animals [J]. J Dalian Fish Univ, 2007, 22(4): 294 298. [2],,. [J]., 2008, 24 (6): 491 496. Qu ZN, Li CJ, Zhao SJ. Study on Eliminate of Malachite Green and its Metabolite in Turbot Muscle [J]. Chin Agr Sci Bull, 2008, 24 (6): 491 496. [3],,. [J]., 2008, 27(8): 430 432. Li HX, Na GS, He W. Advances in Studies on Malachite Green and Leucomalachite Green [J]. Fish Sci, 2008, 27(8): 430 432. [4],,. [J]., 2006, 36(5): 745 748. Qiu XJ, Lin H, Wang LZ. Study on Metabolism of Malachite Green in Crucian (Carassius auratus ) Muscle [J]. Period Ocean Univ China, 2006, 36(5): 745 748. [5] Liewes E, Haenen O. The veterinary approach to eels [M]. BROWN L. Aquaculture for Veterinarians: Fish Husbandry andmedicine. Pergamon, New York, 1993: 311 326. [6] Scott P. Therapy in aquaculture [M]. ROWN L. Aquaculture for Veterinarians: Fish Husbandry and Medicine. Pergamon, NewYork, 1993: 131 152. [7]. [J]., 2009, 2(1): 21 24. Yu PJ. Degradation of Malachite Green in the Fishery Water by Medicine [J]. J Hydroecol, 2009, 2(1): 21 24. [8],,. [J]., 2007, 31 : 104 108. Gao LJ, Cai YQ, Jiang CJ. Accumulation and elimination of malachite green and its primarymetabolite in juvenile European eels (Anguilla anguilla) muscle [J]. J Fish of China, 2007, 31(suppl): 104 108. ( 责 任 编 辑 : 张 宏 梁 ) 作 者 简 介 陈 永 平,, E-mail: yongping008@yahoo.com.cn