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1 4 4 Vol. 4 No Journal of Food Safety and Quality Aug., 董建伟 *, 杨军亭, 侯清娥, 付宏岐, 蒋宝, 薛萍 (, ) 摘要 : 目的 - 方法 (MG), (MAA), (EGDMA),, 结果 μg/l 86.3% 92.1% 83.5% 90.3% 结论, 关键词 : ; ; ; Determination of malachite green in environmental water samples by spectrophotometry with molecularly imprinted solid phase extraction DONG Jian-Wei *, YANG Jun-Ting, HOU Qing-E, FU Hong-Qi, JIANG Bao, XUE Ping (Weinan Vocational and Technical College, Weinan , China) ABSTRACT: Objective To establish a method for determination of malachite green in water samples by spectrophotometry with molecularly imprinted solid phase extraction. Methods The solid phase extraction column was made using molecularly imprinted polymer as filler. The molecularly imprinted polymer was prepared by bulk polymerization using malachite green (MG) as template, methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as cross linking agent. The extraction conditions, such as sample solvents, drying methods, and elution solvents, were optimized. MG in tap and river water samples were detected by spectrophotometer under the optimized conditions. Results The recoveries were in a range of 86.3% 92.1% and 83.5% 90.3% respectively when the spiked concentration in tap and river water samples in the range of μg/l. Conclusion The method is simple, sensitive and it is suitable for the detection of malachite green in environmental water. KEY WORDS: malachite green; molecularly imprinted polymer; solid phase extraction; spectrophotometer 基金项目 : (WZYY201315) Fund: Supported by College-Level Research Projects of Weinan Vocational and Technical College (WZYY201315) * 通讯作者 :,, dongjianwei1305@163.com *Corresponding author: DONG Jian-Wei,Teaching Assistant, Weinan Vocational and Technical College, West of Shengli Street, High-Tech District, Weinan , China. dongjianwei1305@163.com

2 4, : 引言 (malachite green, MG),, [1], [2-5], [6],,, MG (HPLC) [7-8] (LC-MS) [9-12],, [13-14], [7,15],, (molecularly imprinted technology),,, ;,,,,, - 2 材料与方法 2.1 实验材料 (MG)(bright green, BG) (crystal violet, CV) (methyl violet, MV), ; (methacrylic acid, MAA) (ethylene glycol dimethacrylate, EGDMA) Sigma ; (azobisisobutyronitrile, AIBN) ; ;, AL-204 ( -); SY-1-2 ( ); ( ); TLL-C ( ); TDL-80-2B ( ); KQ-200KDV ( ); TU-1901 ( ) 2.2 实验方法分子印迹固相萃取柱的制备 g MG 10 ml, 0.34 ml MAA 5 ml, 5 min ml EGDMA 40 mg AIBN, 5 min, 12 min, h,, μm /(9/1), MIPs,, MIPs ( ), 24 h(48, 0.1 MPa) (NIPs) MIPs,, MIPs NIPs 300 mg MIPs NIPs 2 ml (7.7 cm 0.8 cm i.d.),, (MIPs- NIPs-SPE), 固相萃取条件优化 ( ), 5 ml /(9/1) 5 ml 4 ml, 1 ml/min, MG 2000 μg/l, 2 ml, 1 ml/min, 2 ml 12 h, MG

3 测定量回收率 = 100% 初始量 MG, MG μg/l MG 5 ml, ( 0.5% 10% ) 1 ml 10 ml Eppendorf, (25, 0.08 MPa) 35 Eppendorf 0.5 ml, 15 min, 5 min, Eppendorf MG, / (v/v) (0% 0.25% 0.5% 0.75% 1%), 5 ml / (9/1) 5 ml 4 ml, 1 ml/min 2 ml 1000 μg/l MG, 3 ml, 3 ml /(9/1) 1 ml/min,,, 0.5 ml, MIPs-SPE 重复再生性评价,, 5 ml /(9/1) 5 ml 4 ml, 1 ml/min 2 ml 1000 μg/l MG, 3 ml, 3 ml /(9/1) 1 ml/min,,, 8 8, 0.5 ml, 实际样品的测定,,, μg/l, 20 ml, 0.45 μm,,, (n=3) 3 结果与分析 3.1 确定最大吸收波长 1000 μg/l, nm, 618 nm, 618 nm, C μg/l A, A= C(μg/L)+0.002, R= 固相萃取条件优化上样溶剂选择,,, MG, 1 1, MG 12 h,, ; MG,,,, ( 2), 1 MG Fig. 1 The stability of MG in the different solvents

4, : - 1203 Fig. 2 2 The penetration rate of sample volume using different solvents 3.2.2 干燥方式选择 MG,, 25, 50%,, MG 3 4, 35 25 10%, 35 25, 10% 25 50%, 25, MG 35 25 35 20 min, 25 6 7 MG 40, MG, 25, ( 5) : 35 25, 35 35 3.

4 4, : Fig. 2 2 The penetration rate of sample volume using different solvents 干燥方式选择 MG,, 25, 50%,, MG 3 4, %, 35 25, 10% 25 50%, 25, MG min, MG 40, MG, 25, ( 5) : 35 25, 淋洗液选择 3 25 Fig. 3 Recoveries of malachite green using vacuum dry at 25

1204 4 4 35 Fig. 4 Recoveries of malachite green using nitrogen stream dry at 35, NIPs MIPs 6, NIPs MG, MIPs MG 1%, NIPs 90% MG, MIPs 5% MG, 0.75%, NIP 70% MG, 1.25%, MIP 10% MG,, 1% Fig.

5 Fig. 4 Recoveries of malachite green using nitrogen stream dry at 35, NIPs MIPs 6, NIPs MG, MIPs MG 1%, NIPs 90% MG, MIPs 5% MG, 0.75%, NIP 70% MG, 1.25%, MIP 10% MG,, 1% Fig. 5 5 The total recoveries of malachite green with different drying methods MG NIPs, MIPs, MIPs, ( ),, ;, NIPs MIPs 2 ml 1000 μg/l MG, 3 ml 3.3 MIPs-SPE 再生性评价, 8 7 7, MIPs-SPE 8, 3.4 实际样品测定 1 1 : -, μg/l,

6 4, : , - 4 讨论 MG,,,, Fig. 6 Table 1 6 MG Effect of elution conditions on the recovery of MG in MIP and NIP columns 7 MIPs-SPE Fig. 7 Reproducibility of the MIPs-SPE 表 1 水样加标检测回收率 (n=3) Recoveries of water spiked with MG(n=3) (μg/l) (μg/l) (%) 参考文献 [1] Li YH, Yang T, Qi XL, et al. Development of a group selective molecularly imprinted polymers based solid phase extraction of malachite green from fish water and fish feed samples [J]. Anal Chim Acta, 2008, 624: [2] Annalaura S, Carlo N, Isabella A. Effects of malachite green (MG) and its major metabolite, leucomalachite green (LMG), in two human cell lines [J]. Toxicol Vitro, 2005, 19: [3] Culp SJ, Blankenship LR, Kusewitt DF, et al. Toxicity and metabolism of malachite green and leucomalachite green during short-term feeding to Fischer 344 rats and B6C3F1mice [J]. Chem Biol Interact, 1999, 122: [4] Fernandes C, Lalitha VS, Rao KVK. Enhancing effect of malachite green on the development of hepatic pre-neoplastic lesions induced by N-nitrosodiethylamine in rats [J]. Carcinogenesis, 1991, 12: [5] Shivaji S, Ranjana S, Roy D. Toxicological effects of malachite green [J]. Aquat Toxicol, 2004, 66: [6] Tao YF, Chen DM, Chao XQ, et al. Simultaneous determination of malachite green, gentian violet and their leuco-metabolites in shrimp and salmon by liquid chromatography etandem mass spectrometry with accelerated solvent extraction and auto solid-phase clean-up [J]. Food Contr, 2011, 22, [7],,,. [J]., 2012, 28(4): Hong B, Yuan XP, Wan YW, et al. Simultaneous determination of malachite green and crystal violet residues in water [J]. Food Mach, 2012, 28(4): [8],,,. [J]., 2007, 24(8): Gui YA, Ma L, Wang D, et al. Determination of malachite green in water by high performance liquid chromatography [J]. J Envi-

1206 4 ron Health, 2007, 24(8): 633 634. [9] Geraldine D, Patrick PJ, Mulder CD, et al.

7 ron Health, 2007, 24(8): [9] Geraldine D, Patrick PJ, Mulder CD, et al. Confirmatory analysis of malachite green, leuco-malachite green, crystal violet and leucocrystal violet in salmon by liquid chromatography-tandem mass spectrometry [J]. Anal Chim Acta, 2007, 586, [10] Arroyo D, Ortiz MC, Sarabia LA, et al. Advantages of PARAFAC calibration in the determination of malachite green and its metabolite in fish by liquid chromatography tandem mass spectrometry [J]. J Chromatogr A, 2008, 1187: [11] Lee JB, Kim HY, Jang YM, et al. Determination of malachite green and crystal violet in processed fish products [J]. Food Addit Contam: Part A, 2010, 7: [12] Martinez BMJ, Herrera S, Ucles A, et al. Determination of malachite green residues in fish using molecularly imprinted solid-phase extraction followed by liquid chromatography-linear ion trap mass spectrometry [J]. Anal Chim Acta, 2010, 665, [13],,. [J]., 2002, 11: Guo DH, Ye CL, Zhu YJ. Determination of malachite green in eel by liquid chromatography [J]. Chem Anal Meter, 2002, 11: [14],,,. - [J]., 2011, 8: Mo L, Yang YC, Han J, et al. Determination of malachite green in environmental water samples by spectrophotometry with dispersive liquid-liquid microextraction [J]. Chin J Spectrosc Lab, 2011, 8: [15],,. [J]., 2005, 26: Qiu XJ, Lin H, Jiang J. Research advances on determination of fishery medicine malachite green and their analogs [J]. Mar Fish Res, 2005, 26: 作者简介 ( 责任编辑 : 张宏梁 ) 董建伟, 助教, 主要研究方向为食品污染物检测 dongjianwei1305@163.com

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0.

DOI /j.issn Food Research And Development UPLC-MS/MS 5 0. 118 217 5 38 1 DOI 1.3969/j.issn.5-6521.217.1.28 Food Research And Development 1 2 1 2 1 2 1 2 1 2 1 2 1. 731 2. 731 - UPLC-MS/MS 5. 1 mol/l ProElut PXC 5 % - Thermo Hypersil Gold mm 2.1 mm 1.9 μm ESI