【摘要】：本文針對酪胺和色胺建立了4種電化學(xué)檢測方法,并成功應(yīng)用于實際樣品的檢測,主要內(nèi)容如下:(1)利用循環(huán)伏安法在玻碳電極(GCE)表面通過電化學(xué)聚合形成聚鄰氨基酚膜,對聚合膜進行過氧化處理后得到過氧化聚鄰氨基酚修飾電極,對電極的修飾方法和酪胺的測定條件等進行優(yōu)化。并用掃描電子顯微鏡和交流阻抗法對該電極進行了表征。最后采用方波伏安法對米醋中酪胺的含量進行測定。結(jié)果表明,將GCE置于0.01mol/L鄰氨基酚的高氯酸溶液(0.3 mol/L)中,在-0.5~1.5V電位范圍內(nèi)循環(huán)伏安掃描14圈,將得到的聚鄰氨基酚修飾電極在無水乙醇和超純水中各超聲1 min,然后在0.09mol/L NaOH溶液中于-0.15~1.0V電位范圍內(nèi)循環(huán)伏安掃描16圈,得到的修飾電極在測定酪胺時具有靈敏的響應(yīng)。酪胺的氧化峰電流與其濃度在1.0×10~(-7)~1.0×10~(-5) mol/L和1.0×10~(-5)~2.0×10~(-4) mol/L范圍內(nèi)分別呈良好的線性關(guān)系,檢出限(S/N=3)為5.4×10~(-8)mol/L。將該修飾電極應(yīng)用于米醋樣品中酪胺的測定,并采用高效液相色譜法(HPLC)進行了方法驗證。該修飾電極制作簡單、成本低、檢測速度快,適用于米醋樣品中酪胺含量的測定。(2)利用電流-時間曲線法在GCE表面通過恒電位聚合形成聚吡咯膜,對聚合膜進行過氧化處理后得到過氧化聚吡咯修飾電極,優(yōu)化了該修飾電極對酪胺的測定參數(shù)及評估了該電極的各項性能指標。利用循環(huán)伏安法、交流阻抗法和掃描電子顯微鏡對該修飾電極進行了表征。最后用方波伏安法對酪胺進行測定。結(jié)果表明:GCE在含0.01 mol/L吡咯和0.1 mol/L HNO3的磷酸緩沖溶液中,于0.7V電位下聚合300s,然后在0.2 mol/L NaOH溶液中于-0.2~0.8V電位范圍內(nèi)循環(huán)伏安掃描10圈,得到的修飾電極在測定酪胺時具有較高的靈敏度。酪胺在該電極上的氧化電流與其濃度在8.0×10~(-8)~3.0×10~(-6) mol/L和3.0×10~(-6)~1.5×10~(-4) mol/L范圍內(nèi)呈線性關(guān)系。檢出限(S/N=3)為1.6×10~(-8) mol/L。應(yīng)用該電極對兩種白酒樣品進行檢測,并采用HPLC進行驗證測定。該修飾電極制備簡單,成本低,且具有良好的重復(fù)性、穩(wěn)定性和選擇性,可用于市售白酒中酪胺含量的測定。(3)利用膠體金/粘土(AuCS/Clay)復(fù)合物對GCE進行修飾,得到對色胺具有較高電流響應(yīng)的修飾電極(AuCS/Clay/GCE)。優(yōu)化了該修飾電極測定色胺的方法和條件,利用掃描電子顯微鏡對該修飾電極進行了表征,并對修飾電極的選擇性和重現(xiàn)性等電化學(xué)性能進行評估。然后采用電流-時間曲線法對色胺進行測定。色胺在AuCS/Clay/GCE上的氧化電流與其濃度在4.2×10~(-8)~1.4×10~(-5) mol/L范圍內(nèi)呈良好的線性關(guān)系,檢出限(S/N=3)為1.8×10~(-8)mol/L。進一步基于絲網(wǎng)印刷電極(PK-SPE),采用方波伏安法對色胺進行測定,得到色胺的氧化電流與其濃度在1.0×10~(-7)~5.0×10~(-5)mol/L范圍內(nèi)呈良好的線性關(guān)系,檢出限(S/N=3)為3.3×10~(-8) mol/L。最后對米醋等樣品中的色胺含量進行測定,并用HPLC進行了方法驗證。AuCS/Clay/GCE修飾電極制作簡單,測試靈敏度高,但比PK-SPE的檢測時間長。用PK-SPE測定時樣品用量少(50μL),檢測速度快,選擇性好,兩種方法均可用于市售米醋等樣品中色胺含量的測定。
[Abstract]:In this paper, four electrochemical methods for the determination of tyramine and tryptamine were established and successfully applied to the detection of real samples. The main contents are as follows: (1) Poly (o-aminophenol) film was formed on the surface of glassy carbon electrode (GCE) by cyclic voltammetry. The poly (o-aminophenol) modified electrode was prepared by peroxidation of the film. The electrode was characterized by scanning electron microscopy and alternating current impedance spectroscopy. The content of tyramine in rice vinegar was determined by square wave voltammetry. The results showed that GCE was placed in 0.01 mol/L o-aminophenol perchloric acid solution (0.3 mol/L) at - 0.5-1.5 V potential. Cyclic voltammetry was used to scan 14 cycles in the range of - 0.15 V to 1.0 V. The results showed that the modified electrode had a sensitive response to the determination of tyramine. The modified electrode was applied to the determination of tyramine in rice vinegar samples by high performance liquid chromatography (HPLC). The modified electrode was characterized by simple fabrication, low cost, low detection limit (S/N=3) and good linear relationship in the range of 1.0 (-7) ~1.0 (-5) and 1.0 (-5) ~2.0 (-4) mol/L, respectively. (2) Polypyrrole film was formed on the surface of GCE by potentiostatic polymerization using current-time curve method, and the polypyrrole peroxide modified electrode was obtained by peroxidation of the polymer film. The determination parameters of tyramine were optimized and the properties of the electrode were evaluated. The modified electrode was characterized by cyclic voltammetry, alternating current impedance spectroscopy and scanning electron microscopy. Tyramine was determined by square wave voltammetry. The results showed that GCE was polymerized at 0.7V potential in phosphate buffer solution containing 0.01 mol/L pyrrole and 0.1 mol/L HNO3 for 300 seconds, and then in 0.2 mol/L NaOH solution at - 0.2~0.2. The oxidation current of tyramine on the modified electrode is linearly related to its concentration in the range of 8.0 (-8) (-6) mol/L and 3.0 (-6) (-4) mol/L. The detection limit (S/N=3) is 1.6 65507 The modified electrode has the advantages of simple preparation, low cost, good repeatability, stability and selectivity, and can be used for the determination of tyramine content in liquor. (3) GCE was modified by colloidal gold/clay (AuCS/Clay) complex to obtain high electricity for tryptamine. Modified current-responsive electrode (AuCS/Clay/GCE). The method and conditions for the determination of tryptamine were optimized. The modified electrode was characterized by scanning electron microscopy (SEM). The selectivity and reproducibility of the modified electrode were evaluated. Then the current-time curve method was used to determine tryptamine. Clay/GCE has a good linear relationship between oxidation current and its concentration in the range of 4.2 (-8) ~ 1.4 (-5) mol/L. The detection limit (S/N=3) is 1.8 (-8) mol/L. Based on the screen printed electrode (PK-SPE), the oxidation current and its concentration in the range of 1.0 (-7) ~ 5.0 (-5) mol/L were determined by square wave voltammetry. The detection limit (S/N=3) was 3.3 (-8) mol/L. Finally, the content of tryptamine in rice vinegar and other samples was determined and validated by HPLC. The AuCS/Clay/GCE modified electrode was simple to make and had high sensitivity, but the detection time was longer than that of PK-SPE. The two methods can be used for the determination of the content of the color amine in rice vinegar and other samples.
【學(xué)位授予單位】：仲愷農(nóng)業(yè)工程學(xué)院
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TS207.3;O657.1

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