邻苯二甲酸二甲酯上转换荧光标记检测方法

发布时间：2019-02-12 09:22

【摘要】：本实验以邻苯二甲酸二甲酯为目标物,以上转换荧光纳米材料NaYF4: Er3+,Yb3+(UCNPs)为荧光信号载体,磁性纳米微球为分离载体,建立了一种检测塑化剂邻苯二甲酸二甲酯(DMP)的上转换纳米材料标记磁分离荧光免疫分析方法,并将其应用到食品中邻苯二甲酸二甲酯的检测。采用戊二醛法制备邻苯二甲酸二甲酯包被原(DMP-OVA)。利用水热法合成了粒径均匀的疏水性上转换荧光纳米材料(OA-UCNPs)。通过配体交换法将疏水性上转换荧光纳米材料进行表面羧基修饰制备水溶性上转换荧光纳米材料(PAA-UCNPs)。利用活化酯方法制备得到荧光信号探针和感应探针。经优化,感应探针、信号探针和邻苯二甲酸二甲酯标准品(或待测样品)的添加量均为100μL,反应时间为50 min。在此基础上建立了邻苯二甲酸二甲酯的上转换荧光标记磁分离免疫分析方法,其方法检测限为1 ngmL-1,线性范围为1～1000 ngmL-1。方法与其他17种邻苯二甲酸二甲酯的结构类似物无交叉反应。方法的样品前处理步骤简单,白酒和饮料样品用样品稀释液稀释5倍后可直接用于方法检测,蔬菜样品经简单提取处理后再用样品稀释液稀释5倍后用于检测。三种蔬菜样品(菜花、角瓜、圆白菜)、四种果汁饮料样品(运动饮料、茶饮料、含乳饮料、芒果汁)和三种不同度数的白酒样品(42°、56°、62°)(经GC-MS检测不含有邻苯二甲酸二甲酯)在10,100, 00 ng g-1(ng mL-1)的添加水平下的回收率在79.1%～124.0%之间。所建立的方法的测定结果与GC-MS方法的测定结果之间有很好的相关性(R2=0.9721)。本研究建立的邻苯二甲酸二甲酯(DMP)的上转换纳米材料标记磁分离荧光免疫分析方法灵敏度高,特异性好,样品前处理方法简单,受基质干扰小,易于操作,适用于食品样品中邻苯二甲酸二甲酯的快速定量检测。
[Abstract]:In this experiment, dimethyl phthalate was used as the target material, NaYF4: Er3, Yb3 (UCNPs) as fluorescent signal carrier and magnetic nanospheres as separation carrier. A method for the detection of dimethyl phthalate (DMP) by upconversion nano-material labeled magnetic separation fluorescence immunoassay (FIA) was established and applied to the detection of dimethyl phthalate in food. Dimethyl phthalate (DMP-OVA) was prepared by glutaraldehyde method. Hydrophobic up-conversion fluorescent nanomaterials (OA-UCNPs) with uniform particle size were synthesized by hydrothermal method. Surface carboxyl modification of hydrophobic up-conversion fluorescent nanomaterials (PAA-UCNPs) was carried out by ligand exchange method. Fluorescence signal probe and inductive probe were prepared by activation ester method. After optimization, the addition amount of induction probe, signal probe and dimethyl phthalate standard (or sample to be tested) is 100 渭 L and the reaction time is 50 min.. On the basis of this, an up-conversion fluorescence labeling method for magnetic separation and immunoassay of dimethyl phthalate was established. The detection limit of the method was 1 ngmL-1, and the linear range was 11000 ngmL-1.. Methods there was no cross-reaction with the other 17 structural analogs of dimethyl phthalate. The sample pretreatment procedure of the method is simple. The samples of liquor and beverage can be directly used for detection after dilution with sample diluent for 5 times, and vegetable samples can be used for detection after simple extraction and then dilution with sample diluent for 5 times. Three kinds of vegetable samples (cauliflower, cantaloupe, cabbage), four kinds of juice drink (sports drink, tea drink, milk drink, mango juice) and three kinds of liquor samples with different degrees (42 掳, 56 掳), The recoveries of dimethyl phthalate were between 79.1% and 124.0% at the addition level of 10m 100,00 ng g -1 (ng mL-1) (determined by GC-MS without dimethyl phthalate). There is a good correlation between the results of the established method and that of GC-MS method (R2O0.9721). In this study, the upconversion nanomaterial labeled fluorescence immunoassay for dimethyl phthalate (DMP) was developed, which was characterized by high sensitivity, good specificity, simple sample pretreatment, little interference by matrix, and easy operation. It is suitable for rapid quantitative determination of dimethyl phthalate in food samples.
【学位授予单位】：天津科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS207.3;O657.3

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