【作者】 邓凯芬；

【导师】 李忠海； 胡叶碧；

【作者基本信息】 中南林业科技大学 ， 农产品加工及贮藏工程， 2012， 硕士

【摘要】 因与食品直接接触,食品包装的安全性越来越受到关注。有些不法商贩因利益驱使,以废旧纸料为原料进而生产食品包装用纸,甚至直接将荧光物质涂布在食品包装纸上。荧光增白剂通过接触有可能进入食品中。荧光增白剂易与伤口处蛋白质结合,过量接触还会有潜在的致癌作用。虽然各国标准明确规定食品包装禁用荧光增白剂,但是目前国内外对其检测的研究较少,鉴于荧光增白剂对人体的危害,建立快速、准确和灵敏的提取检测方法势在必行。由于包装与食品直接接触,包装中的有害物质可能迁移到食品中,食用后极易对人体产生危害。而食品基体具有复杂和多样性,国内外大都采用食品模拟物替代食品进行迁移实验。由于迁移物质在食品模拟液的不稳定性会引起迁移实验结果的准确性和相关的毒理性问题,因此迁移物质的稳定性日益受到重视。本实验以纸塑食品包装为研究对象,对其所含的3种荧光增白剂VBL、VBA、APC的高效液相色谱方法进行研究,得其高效液相色谱方法为：采用月旭AQ-C18(4.6x250mm,5μm)色谱柱,荧光检测器激发波长362nm、发射波长430nm,柱温35℃；以水和甲醇为流动相,流速1.0mL/min,进样量10μL,梯度洗脱程序如下：初始流动相甲醇：水=25：75；到3.00min,甲醇：水=65：35；到4.00min,甲醇：水=65：35；到5.00min,甲醇：水=95：5；到10.00min,甲醇：水=95：5。本实验通过单因素实验和正交试验得到了加速溶剂萃取法提取纸塑包装中荧光增白剂VBL的最佳提取条件为：提取溶剂N,N-二甲基乙酰胺(DMF)、静态萃取时间7min,冲洗体积75%,循环次数3次,静态萃取温度110℃。方法学考察实验结果表明目标物VBL在浓度0.1-10.0μg/mL范围内,线性良好,相关系数为0.9999；加标回收率实验表明在三个添加水平下平均回收率89.86%-91.40%之间,相对标准偏差(RSD)为2.07%-2.18%,方法准确可靠,有望用于食品纸塑包装中荧光增白剂VBL的定量检测。本实验通过研究荧光增白剂VBL、 VBA、 APC在蒸馏水、20%乙醇、50%乙醇、95%乙醇、3%乙酸、正己烷、异辛烷的溶解性后确定了荧光增白剂迁移实验的模拟液为蒸馏水、20%乙醇、50%乙醇、95%乙醇,进一步研究了三个迁移温度下三种荧光增白剂在四种迁移模拟物中的稳定性,确定了三种荧光增白剂的迁移条件。本实验进行了常温下食品纸塑包装中荧光增白剂VBL在蒸馏水、20%乙醇、50%乙醇、95%乙醇四种模拟液的迁移实验,实验结果表明,三种荧光增白剂迁移时间越长,迁移量增加；模拟液的选择不同,荧光增白剂迁移量不同；此外迁移量也与污染物的初始浓度以及污染物分子量有关。更多还原

【Abstract】 Because of contacting with food directly, the security of food packaging are took more and more attentions. Due to profit-driven, some unscrupulous traders use waste paper materials as raw materials to make food packaging paper again or even paint fluorescent substance in food wrappers directly. Fluorescent whitening agent may enter the food through contact. Fluorescent whitening agent can combine with the protein of the body wound or even lead to the potential carcinogenic effects if excessive exposure. Although national standards explicitly require that addition of the fluorescent whitening agent to food packaging are disable, but the method to detect fluorescent whitening agent are less. As a result, quickly, accurately and sensitively extraction detection is necessary.As food packaging are always contacted with food, so the hazardous substances of food packaging which can do harm to body may migrate to food. Because of the complexity and diversity of the food matrix, most of the food stimulants are instead of food to do the migration experiment. For the instability of Migration of substances in food stimulants will cause the accuracy of the migration experimental results and relevant toxicological issues, so migration stability of the substance are get more attention.In the experiment, we use paper and plastic food packaging to study three kinds of fluorescent whitening agents including VBL, VBA and APC by high performance liquid chromatographic (HPLC) method.HPLC conditions are as follows:ultimate C18(chromatographic column4.6×250mm,5μm), ethanol:water (90:10)(mobile phase), fluorescence detector (λexcitation=362nm, λemission=430nm),1.0ml/min (flow rate),35℃(column temperature) and10μL (injection volume). The conditions of the accelerated solvent extraction were optimized using both single factor experiment and orthogonal experiment and the results showed that the optimum extraction conditions were as follows:7min (extraction time),70%(flushed volume),3(cycle-index) and110℃(Extraction temperature).It gets the optimum extraction conditions for accelerated solvent extraction microwave-assisted extraction through single-factor experiments and orthogonal test using N, N-dimethyl formamide (DMF) as solvent. The methodology inspection experimental results show that the accelerated solvent extraction-HPLC has good linearity in the range of target0.1-10.0μg/mL with correlation coefficient of0.9999; Three levels, average recovery is89.86%~91.40%, relative standard deviation (RSD) are as low as2.07%-2.18%.In the study, we have researched fluorescent brighteners including VBL, VBA and APC in distilled water,20%ethanol,50%ethanol,95%ethanol,3%acetic acid, hexane, isooctane solubility. We set the migration experiment simulated body fluid for distilled water,20%ethanol,50%ethanol,95%ethanol. We study the stability of the three fluorescent brighteners in three migration temperature and in the four migration mimics identified so that three fluorescent brightener migration conditions are determined.For convenience, this experiment is carried out at room temperature to study simulated body fluid migration experiment of fluorescent whitening agent VBL in distilled water,20%ethanol,50%ethanol and95%ethanol in food paper and plastic packaging. The experimental results show that, migration increases following migration time; different simulation,different migration; initial concentration and molecular also accounts for migration.更多还原