HPLC Determination of 6 Aromatic Amines Migrated from Food Contacting Materials with Extraction by Ionic Liquid
摘 要
提出了用高效液相色谱法测定食品接触材料中4,4′-二氨基二苯基甲烷、2,4-二甲基苯胺、4-氯邻甲苯胺、4-氨基联苯、3,3′-二氯联苯胺、4-氨基偶氮苯等6种芳香胺迁移量的测定方法。向样品的水浸泡液或乙酸(3+97)溶液浸泡液25.0 mL中加入离子液体[C6mim][PF6] 0.652 3 g作为萃取剂,用磷酸盐缓冲溶液或氨水调至pH 8,加入氯化钠1.25 g,涡旋振荡萃取5 min,随后再离心5 min,下层离子液体相供高效液相色谱分析。用Diamonsil C18色谱柱作固定相,流动相为水和乙腈混合溶液,于波长235 nm处进行检测。6种芳香胺的线性范围为0.02~2.0 mg·L-1,检出限(3S/N)在4.0~10.0 μg·L-1之间。方法用于尼龙勺样品分析,并以此为基体进行加标回收试验,测得回收率在91.6%~106%之间,测定值的相对标准偏差(n=5)在1.4%~8.8%之间。
Abstract
A method of HPLC for the determination of 6 aromatic amines, i.e., 4,4′-methyenedianiline, 2,4-dimethylaniline, 4-chloro-o-toluidine, 4-aminobiphenyl, 3,3′-dichlorobenzidine and 4-aminoazobenzene migrated from food contacting materials was proposed. The sample was soaked in 25.0 mL of water or acetic acid solution (3+97). The soaking solution was mixed with 0.652 3 g of ionic liquid [C6mim][PF6] which is used as extractant. Acidity of the mixture was adjusted to pH 8 with PBS or aq. ammonia. After addition of 1.25 g of NaCl, the mixture was extracted by vortical shaking for 5 min, and then centrifuged for 5 min, the lower ionic liquid phase was taken and used for HPLC analysis. Diamonsil C18 column was used as the stationary phase and mixtures of water and acetonitrile used as mobile phase. Detection was made at the wave length of 235 nm. Linearity ranges of 6 the aromatic amines were between 0.02-2.0 mg·L-1. The limits of detection (3S/N) found were from 4.0 to 10.0 μg·L-1. The proposed method was applied to the analysis of a sample of Nylon spoon, and recovery was tested by standard addition method, giving values of recovery and RSD′s (n=7) in the ranges of 91.6%-106% and 1.4%-8.8% respectively.
中图分类号 O652.63
所属栏目 工作简报
基金项目 国家质监总局项目(2011IK036);宁波市自然基金项目(2010A610011)
收稿日期 2013/1/8
修改稿日期
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备注朱晓艳(1978-),女,浙江兰溪人,高级工程师,主要从事食品接触材料检测方法研究。
引用该论文: ZHU Xiao-yan,CAO Guo-zhou,XIAO Dao-qing,WU Qian. HPLC Determination of 6 Aromatic Amines Migrated from Food Contacting Materials with Extraction by Ionic Liquid[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(10): 1188~1192
朱晓艳,曹国洲,肖道清,吴倩. 离子液体萃取-高效液相色谱法测定食品接触材料中6种芳香胺的迁移量[J]. 理化检验-化学分册, 2013, 49(10): 1188~1192
被引情况:
【1】王海婷,吴 婷,施超欧,贺 冰,陈爱连,缪文彬, "高效液相色谱法测定模拟食品接触材料中3,3′-二氯-4,4′-二氨基二苯基甲烷的迁移量",理化检验-化学分册 51, 1598-1600(2015)
【2】满正印,王全林,李和生,沈坚,张爱芝, "超高效液相色谱-串联质谱法测定具色塑料餐具中33种初级芳香胺的残留量和迁移量",理化检验-化学分册 52, 1142-1149(2016)
【3】孙多志,左莹,禄春强,韩陈,秦紫明, "液相色谱-串联质谱法测定复合塑料食品包装袋中的二氨基甲苯",理化检验-化学分册 52, 52-55(2016)
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参考文献
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【3】BHASKAR M, ARUNA P, JEEVAN R, et al. β-Cyclodextrin-polyurethane polymer as solid phase extraction material for the analysis of carcinogenic aromatic amines[J]. Anal Chim Acta, 2004,509(1):39-45.
【4】COMMISSION DIRECTIVE 2007/19/EC of 30 March 2007, amending Directive 2002/72/EC relating to plastic materials and articles intended to come into contact with food and Council Directive 85/572/EEC laying down the list of simulants to be used for testing migration of constituents of plastic materials and articles intended to come into contact with foodstuffs[S].
【5】COMMISSION DIRECTIVE 2002/72/EC of 6 August 2002, relating to plastic materials and articles intended to comein to contact with foodstuff[S].
【6】陈志锋,刘晓华,孙利.高效液相色谱法测定复合塑料食品包装中初级芳香胺的迁移量[J].包装工程, 2010,31(3):48-51.
【7】肖道清,陈少鸿,朱晓艳,等.固相萃取/气相色谱一质谱法对接触食品的塑料制品中24种芳香族伯胺迁移量的同时测定[J].分析测试学报, 2008,28(10):1155-1159.
【8】BOUZIGE M, MACHTALRE G, LEGEAY P, et al. Quantitative determination of 22 primary aromatic amines by cation-exchange solid-phase extraction and liquid chromatography-mass spectrometry[J]. J Chromatogr A, 2009,1216(27):5176-5181.
【9】BOUZIGE M, MACHTALRE G, LEGEAY P, et al,New methodology for a selective on-line monitoring of some polar priority industrial chemicals in waste water[J]. Waste Management, 1999,19(2):171-180.
【10】LIN Zian, ZHANG Jian-hua, CUI Hui-min, et al. Determination of aromatic amines in environmental water sample by hollow ?ber-liquid phase microextraction and microemulsion electrokinetic chromatography[J]. J Chromatogr A, 2010,1217(26):4507-4510.
【11】ZENG Zhao-rui, QIU Wen-li, YANG Min et al. Solid-phase microextraction of monocyclic aromatic amines using novel fibers coated with crown ether[J]. J Chromatogr A, 2001,934(1):51-57.
【12】FU X M, DAI S G, ZHANG Y. 1-Butyl-3-methylimidazolium hexafluorophosphate ionic liquid-based liquid-liquid microextraction for the determination of 4-nonylphenol and 4-tertoctylphenol in environmental waters[J]. Intern J Environ Anal Chem, 2006,86(13):985-993.
【13】丁健桦,何海霞,林海禄,等.离子液体-液相微萃取-高效液相色谱法测定纺织品中芳香胺[J].分析化学, 2008,36(12):1662-1666.
【14】陆娜萍,李在均,李继霞,等.室温离子液体萃取石墨炉原子吸收光谱法测定超痕量钼[J].冶金分析, 2008,28(7):28-32.
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