發(fā)布時(shí)間：2019-02-12 09:22

【摘要】：本實(shí)驗(yàn)以鄰苯二甲酸二甲酯為目標(biāo)物,以上轉(zhuǎn)換熒光納米材料NaYF4: Er3+,Yb3+(UCNPs)為熒光信號(hào)載體,磁性納米微球?yàn)榉蛛x載體,建立了一種檢測(cè)塑化劑鄰苯二甲酸二甲酯(DMP)的上轉(zhuǎn)換納米材料標(biāo)記磁分離熒光免疫分析方法,并將其應(yīng)用到食品中鄰苯二甲酸二甲酯的檢測(cè)。采用戊二醛法制備鄰苯二甲酸二甲酯包被原(DMP-OVA)。利用水熱法合成了粒徑均勻的疏水性上轉(zhuǎn)換熒光納米材料(OA-UCNPs)。通過配體交換法將疏水性上轉(zhuǎn)換熒光納米材料進(jìn)行表面羧基修飾制備水溶性上轉(zhuǎn)換熒光納米材料(PAA-UCNPs)。利用活化酯方法制備得到熒光信號(hào)探針和感應(yīng)探針。經(jīng)優(yōu)化,感應(yīng)探針、信號(hào)探針和鄰苯二甲酸二甲酯標(biāo)準(zhǔn)品(或待測(cè)樣品)的添加量均為100μL,反應(yīng)時(shí)間為50 min。在此基礎(chǔ)上建立了鄰苯二甲酸二甲酯的上轉(zhuǎn)換熒光標(biāo)記磁分離免疫分析方法,其方法檢測(cè)限為1 ngmL-1,線性范圍為1～1000 ngmL-1。方法與其他17種鄰苯二甲酸二甲酯的結(jié)構(gòu)類似物無(wú)交叉反應(yīng)。方法的樣品前處理步驟簡(jiǎn)單,白酒和飲料樣品用樣品稀釋液稀釋5倍后可直接用于方法檢測(cè),蔬菜樣品經(jīng)簡(jiǎn)單提取處理后再用樣品稀釋液稀釋5倍后用于檢測(cè)。三種蔬菜樣品(菜花、角瓜、圓白菜)、四種果汁飲料樣品(運(yùn)動(dòng)飲料、茶飲料、含乳飲料、芒果汁)和三種不同度數(shù)的白酒樣品(42°、56°、62°)(經(jīng)GC-MS檢測(cè)不含有鄰苯二甲酸二甲酯)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%之間。所建立的方法的測(cè)定結(jié)果與GC-MS方法的測(cè)定結(jié)果之間有很好的相關(guān)性(R2=0.9721)。本研究建立的鄰苯二甲酸二甲酯(DMP)的上轉(zhuǎn)換納米材料標(biāo)記磁分離熒光免疫分析方法靈敏度高,特異性好,樣品前處理方法簡(jiǎn)單,受基質(zhì)干擾小,易于操作,適用于食品樣品中鄰苯二甲酸二甲酯的快速定量檢測(cè)。
[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 擄, 56 擄), 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.
【學(xué)位授予單位】：天津科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TS207.3;O657.3

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