【摘要】：雙酚A (Bisphenol A, BPA)是一種常見的環(huán)境雌激素，在痕量濃度就可以干擾人體的內(nèi)分泌系統(tǒng)并引發(fā)多種毒性作用；而且BPA在日常生活及工業(yè)生產(chǎn)中的用途非常廣泛，所以簡便、靈敏地監(jiān)測BPA非常重要。在本研究中，我們采用溶膠凝膠法制備了以BPA偽模板分子印跡聚合物(Dummy molecularlyimprinted polymers, DMIPs)為涂層材料的攪拌棒，并應(yīng)用其吸附萃取自來水中痕量的BPA。 攪拌棒吸附萃取技術(shù)(Stir bar sorptive extraction, SBSE)是將對(duì)待測物具有吸附作用的萃取材料涂附在攪拌棒表面，使攪拌棒在自身攪拌的同時(shí)完成對(duì)待測物的富集，具有靈敏度高、溶劑耗費(fèi)少、操作簡便等優(yōu)點(diǎn)。但是現(xiàn)有的市售攪拌棒只有非極性涂層材料，對(duì)極性物質(zhì)吸附能力非常差，而且缺乏特異選擇性。為了克服這一缺陷，我們利用分子印跡聚合物吸附的特異性，采用溶膠凝膠法制備了對(duì)BPA有良好特異吸附作用的BPA偽模板分子印跡攪拌棒(DMIPs攪拌棒)。掃描電鏡圖顯示，BPA偽模板分子印跡涂層具有粗糙、均勻的表面結(jié)構(gòu)，涂層厚度約57μm。DMIPs、聚二甲基硅氧烷涂層和BPA偽模板分子印跡涂層的紅外圖譜表明DMIPs被成功嵌入到凝膠結(jié)構(gòu)中。 選擇性吸附實(shí)驗(yàn)數(shù)據(jù)顯示：在對(duì)含有BPA和BPA結(jié)構(gòu)類似物的混合水溶液進(jìn)行吸附萃取時(shí)，DMIPs攪拌棒對(duì)BPA的回收率分別是聯(lián)苯二酚的3~4倍，是4-叔丁基酚的3~7倍，是四溴雙酚A的61~103倍。這充分表明DMIPs攪拌棒對(duì)BPA具有良好的選擇性吸附能力。此外，DMIPs攪拌棒對(duì)BPA的萃取能力并不隨著混合溶液中BPA結(jié)構(gòu)類似物濃度的增加而下降，而是保持相對(duì)穩(wěn)定(回收率在88~98%之間)，這顯示DMIPs攪拌棒具有較強(qiáng)的抗干擾能力。 同時(shí)，我們比較了DMIPs攪拌棒、以空白印跡聚合物(Non-imprintedpolymers, NIPs)為涂層的攪拌棒(NIPs攪拌棒)和以聚二甲基硅氧烷(Polydimethylsiloxane, PDMS)為涂層的攪拌棒(PDMS攪拌棒)對(duì)BPA的吸附能力。數(shù)據(jù)顯示，DMIPs攪拌棒對(duì)BPA的回收率分別是NIPs攪拌棒的7倍，是PDMS攪拌棒的24倍。顯然，DMIPs攪拌棒對(duì)BPA的吸附能力遠(yuǎn)遠(yuǎn)優(yōu)于其它兩種攪拌棒。 最后，我們優(yōu)化了應(yīng)用DMIPs攪拌棒進(jìn)行吸附萃取的實(shí)驗(yàn)條件，并成功地將DMIPs-SBSE與高效液相熒光檢測法聯(lián)合，，測定了自來水中的BPA。該分析方法的標(biāo)準(zhǔn)曲線在BPA濃度0.0228-0.456 ng mL-1范圍內(nèi)線性良好，相關(guān)系數(shù)為0.9994。BPA的檢測限為5.70 pg mL-1 (S/N=3)。我們應(yīng)用該方法測定了自來水中痕量的BPA，得到了滿意的結(jié)果。BPA加標(biāo)回收率在81.7?98.2%范圍內(nèi)，相對(duì)標(biāo)準(zhǔn)偏差為10.2%。
[Abstract]:Bisphenol A (Bisphenol A, BPA) (BPA) is a common environmental estrogen, which can disturb the endocrine system of human body at trace concentration and induce many toxic effects. BPA is widely used in daily life and industrial production, so it is very important to monitor BPA easily and sensitively. In this study, we prepared the agitator rod using BPA pseudo-template molecularly imprinted polymer (Dummy molecularlyimprinted polymers, DMIPs) as coating material by sol-gel method, and used it to adsorb and extract trace BPA. from tap water. Agitator rod adsorption extraction technology (Stir bar sorptive extraction, SBSE) is a kind of extraction material which can be adsorbed on the surface of agitator rod. The agitator rod has high sensitivity and high sensitivity, which makes the agitator complete the enrichment of the test material while stirring itself at the same time. The solvent consumption is less, the operation is simple and so on. However, the non-polar coating materials are the only available agitator rods, and the adsorption ability of polar materials is very poor, and there is no specific selectivity. In order to overcome this defect, BPA pseudo-template molecular imprinted agitator (DMIPs) was prepared by sol-gel method by using molecular imprinted polymer adsorption specificity. Scanning electron microscopy showed that the BPA pseudo-template molecular imprinted coating had a rough and uniform surface structure, and the coating thickness was about 57 渭 m.DMIPs. The IR spectra of polydimethylsiloxane coating and BPA pseudo-template molecular imprinted coating show that DMIPs is successfully embedded into the gel structure. The experimental data of selective adsorption showed that the recovery of BPA by DMIPs agitator was 3 4 times of that of dihydroxybenzene and 37 times of that of 4 tert-Ding Ji phenol when the mixed aqueous solution containing BPA and BPA analogues was adsorbed and extracted. It is 103 times higher than tetrabromobisphenol A (BPA). This fully indicates that DMIPs agitator has a good selective adsorption capacity for BPA. In addition, the extraction ability of DMIPs agitator for BPA does not decrease with the increase of BPA structure analogue concentration in mixed solution, but remains relatively stable (recovery rate is between 88% and 98%), which indicates that DMIPs stirring rod has strong anti-interference ability. At the same time, we compared the adsorption ability of DMIPs agitator rod, NIPs agitator rod coated with blank imprinted polymer (Non-imprintedpolymers, NIPs) and PDMS agitator rod coated with polydimethylsiloxane (Polydimethylsiloxane, PDMS). The results showed that the recovery of BPA by DMIPs was 7 times of that of NIPs and 24 times of that of PDMS. Obviously, the adsorption ability of DMIPs agitator to BPA is much better than that of other two agitators. Finally, we optimized the experimental conditions of adsorption and extraction with DMIPs agitator, and successfully combined DMIPs-SBSE with high performance liquid phase fluorescence detection method to determine BPA. in tap water. The standard curve was linear in the range of 0.0228-0.456 ng mL-1 for BPA, and the detection limit of 0.9994.BPA was 5.70 pg mL-1 (S/N=3). The method has been applied to the determination of trace BPA, in tap water with satisfactory results. The recoveries of BPA are within the range of 81.7% and 98.2%, and the relative standard deviation is 10.2%.
【學(xué)位授予單位】：南京醫(yī)科大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2011
【分類號(hào)】：TB383.1

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