【摘要】：苯醚甲環(huán)唑是一種被廣泛使用的低毒性殺菌劑。目前,用于檢測食品中苯醚甲環(huán)唑的方法主要有液相色譜法,氣相色譜法,色譜-質(zhì)譜聯(lián)用等分析方法。然而,這些方法均有一些缺點(diǎn),如:檢測耗費(fèi)時間長,所需儀器昂貴,在檢測過程中需要耗費(fèi)大量的溶劑等。因此,建立一種快速、靈敏的苯醚甲環(huán)唑檢測方法具有重要意義。本研究建立了一種基于金納米顆粒及分子印跡的電化學(xué)傳感檢測方法,用于食品中苯醚甲環(huán)唑的檢測。具體方法是,以苯醚甲環(huán)唑?yàn)槟０宸肿?對氨基苯硫酚為功能單體,在修飾有金納米顆粒的玻碳電極表面電沉積分子印跡聚合物膜,從而實(shí)現(xiàn)對苯醚甲環(huán)唑的特異性檢測。一方面,金納米顆�？梢宰鳛樵鰪�(qiáng)電化學(xué)傳感器的電信號材料,增大電極比表面積從而提高電極表面分子印跡聚合物膜的有效印跡位點(diǎn);另一方面,修飾的分子印跡聚合物膜可特異性識別目標(biāo)物苯醚甲環(huán)唑。在實(shí)驗(yàn)中,使用掃描電子顯微鏡,原子力顯微鏡對修飾有金納米顆粒及金納米顆粒-分子印跡膜的玻碳電極進(jìn)行形貌表征,同時用循環(huán)伏安法以及差分脈沖伏安法對工作電極進(jìn)行條件優(yōu)化及電化學(xué)行為表征。最后,對構(gòu)建傳感器的吸附性,選擇性,重復(fù)性,穩(wěn)定性進(jìn)行評價及分析。結(jié)果表明,在優(yōu)化的條件下,構(gòu)建的電化學(xué)傳感器在2×10-6-1.4×10-5molL-1濃度范圍內(nèi)對苯醚甲環(huán)唑呈現(xiàn)較好的電化學(xué)響應(yīng),根據(jù)三倍信噪比(S/N=3)計算,該方法的最低檢出限為9.49×10-7molL-1。此外,構(gòu)建的電化學(xué)傳感器有良好的選擇性、重復(fù)性和穩(wěn)定性。該方法成功地用于食品(白菜,蘋果,桃汁)中苯醚甲環(huán)唑的加標(biāo)回收檢測,用高效液相色譜法驗(yàn)證,兩種方法具有一致性。綜上所述,這種電化學(xué)傳感器能夠?yàn)闄z測食品中的苯醚甲環(huán)唑提供一種新方法。
[Abstract]:Difenoconazole is a widely used fungicides with low toxicity. At present, liquid chromatography, gas chromatography, chromatography-mass spectrometry and other analytical methods are the main methods for the determination of dimethyclozole in food. However, these methods have some disadvantages, such as: the detection takes a long time, the required instruments are expensive, and a large amount of solvents are needed in the detection process. Therefore, it is of great significance to establish a rapid and sensitive method for the determination of dimethylcyclozole. An electrochemical sensing method based on gold nanoparticles and molecular imprinting was developed for the detection of diphenyl ether triazole in food. The specific method is to electrodeposit molecularly imprinted polymer films on the surface of glassy carbon electrode modified with gold nanoparticles using diphenyl ether dioxazole as template molecule and p aminophenol as functional monomer. On the one hand, gold nanoparticles can be used as electrical signal materials to enhance the electrochemical sensor, increase the specific surface area of the electrode and thus improve the effective imprinting site of the molecularly imprinted polymer membrane on the electrode surface. The modified molecularly imprinted polymer membrane can specifically recognize the target of diphenyl ether triazole. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used to characterize the morphology of glassy carbon electrodes modified with gold nanoparticles and molecularly imprinted films. The working electrode was optimized by cyclic voltammetry and differential pulse voltammetry. Finally, the adsorbability, selectivity, repeatability and stability of the sensor were evaluated and analyzed. The results show that the electrochemical sensor has a good electrochemical response to diphenyl ether triazole in the concentration range of 2 脳 10 ~ (-6) to 1.4 脳 10-5molL-1, and the detection limit of the method is 9.49 脳 10 ~ (-7) mol / L ~ (-1), calculated according to the triple signal-to-noise ratio (S/N=3). In addition, the electrochemical sensor has good selectivity, repeatability and stability. The method has been successfully applied to the determination of dioxazole in food (cabbage, apple and peach juice). The two methods are consistent with each other by high performance liquid chromatography (HPLC). In conclusion, this electrochemical sensor can provide a new method for the detection of diphenyl ether triazole in food.
【學(xué)位授予單位】：天津科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TS207.5;TP212.2

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