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作 者:朱晓艳[1] 曹国洲[1] 肖道清[1] 吴倩[1]
出 处:《理化检验(化学分册)》2013年第10期1188-1192,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:国家质监总局项目(2011IK036);宁波市自然基金项目(2010A610011)
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[C_6mim][PF_6]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 C_(18)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4.0~10.0μg·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。A method of HPLC for the delerminadon of 6 aromatic amines, i. e., 4,4-methyenedlamllne, 2. 4-dimethylaniline, 4 ehlorro-o-toluidine, 4-aminohiphenyl, 3,3'- dichlorobenzidine and 4 aminoazoobenzene migrated from food conlacling malerials was proposed. The sample was soaked in 25. 0 mL of waler or acetic acid solution (3+97). The soaking solulion was mixed with 0. 652 3 g of ionic liquid [C6min][PF6] which is used as extractanl. 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 wortical shaking for 5 min, and then centrifuged for 5 min, the lower ionic liquid phase was taken and used for HPLC amlysis. 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. 2Fhe 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.
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