【摘要】：苯甲酸（Benzoic acid；BA）是常用的食品添加劑，由于對食品具有保鮮防腐作用，非法超標(biāo)添加BA的現(xiàn)象時有發(fā)生。過量食用BA影響人體健康，可能誘發(fā)癌癥。BA含量的衛(wèi)生檢測是食品安全評價的重要內(nèi)容之一，加強(qiáng)對BA的衛(wèi)生檢驗十分必要。鄰苯二甲酸二丁酯（Dibutyl phthalate；DBP）是一種塑料增塑劑（Plasticizer），是一種重要的環(huán)境荷爾蒙物質(zhì)；我國和美國國家環(huán)保局（EPA）都將DBP列為環(huán)境優(yōu)先控制有毒污染物。 三聚氰胺（Melamine；MM）通常用于生產(chǎn)三聚氰胺/甲醛樹脂。在人體內(nèi)，MM容易形成難溶性鹽結(jié)晶，導(dǎo)致尿路系統(tǒng)結(jié)石、膀胱上皮增生等，嚴(yán)重危害人體健康。DBP和MM都是重要的工業(yè)原料，是禁用的食品添加物質(zhì)。由于增塑劑對一些食品產(chǎn)品具有特殊的功效，加入MM可虛假提高乳制品的蛋白質(zhì)含量，近年來，DBP和MM都被非法用作食品添加物，引發(fā)了食品安全突發(fā)事件，引起社會強(qiáng)烈反響。檢測食品中的DBP和MM已經(jīng)成為業(yè)內(nèi)和社會高度關(guān)注的食品安全工作，研究建立這三種食品添加物質(zhì)新的檢測方法具有重要衛(wèi)生學(xué)意義。 本文基于Fenton反應(yīng)和共振瑞利散射光譜，研究建立了BA、DBP和MM三種有毒有害物質(zhì)的熒光光譜、或共振瑞利散射光譜檢測新方法，為大面積排查和檢測這三種食品添加物質(zhì)提供了實用的新方法。 本文第二章基于Fenton反應(yīng)建立了苯甲酸的熒光光譜衛(wèi)生檢測新方法。在pH=7.6的近中性環(huán)境中，，以EDTA-Fe2+/H2O2為Fenton試劑，用苯甲酸捕獲Fenton反應(yīng)產(chǎn)生的·OH自由基，形成熒光物質(zhì)羥基苯甲酸。在λex=303nm，λem=414nm，通帶寬度10nm條件下，測定待測溶液的發(fā)射熒光強(qiáng)度，標(biāo)準(zhǔn)曲線法定量檢測食品的苯甲酸。測定7.0×10-5、1.5×10-4和5.0×10-4mol/L三種濃度水平苯甲酸的RSD=0.40%~1.40%；平行測定空白溶液的s=0.035，RSD=3.30%。線性回歸方程為F=98.76c－4.12，（c,×10-4mol/L），r=0.9992。檢出限D(zhuǎn)L=1.06×10-7mol/L；測定下限為3.53×10-7mol/L；測定線性范圍為3.53×10-7~9.0×10-4mol/L。樣品測定回收率P=96.50%~102.50%，RSD=2.66%。新方法的測定線性范圍寬，檢出限低，應(yīng)用廣泛；樣品處理方法簡單，操作簡便，實際樣品測定精密、準(zhǔn)確，測定結(jié)果令人滿意。 本文第三章，F(xiàn)enton反應(yīng)產(chǎn)生羥基自由基（·OH），DBP水解產(chǎn)生鄰苯二甲酸鈉，二者反應(yīng)生成熒光物質(zhì)羥基鄰苯二甲酸鈉，據(jù)此建立了熒光光譜法間接測定樣品中DBP的新方法。在優(yōu)化的反應(yīng)條件下，在2.8×10-7~2.3×10-4mol/L濃度范圍內(nèi)，熒光強(qiáng)度與DBP的濃度之間有良好的線性關(guān)系，其回歸方程為：ΔF=18.47c－11.338（c,10-5mol/L），r=0.9970；方法檢出限為8.4×10-8mol/L，相對標(biāo)準(zhǔn)偏差RSD=1.4%~2.6%；樣品加標(biāo)回收率96.73%~105.68%。方法準(zhǔn)確、靈敏。 本文第四章基于共振瑞利散射光譜的特點，建立了共振瑞利散射光譜測定食品中三聚氰胺的新方法。在pH=5.5的B-R緩沖溶液中，在四氫呋喃介質(zhì)中，三聚氰胺與巴比妥以非共價鍵方式結(jié)合形成聚集體，激發(fā)產(chǎn)生強(qiáng)烈的共振瑞利散射。濃度為3.03×10-8～1.60×10-7mol/L時，體系在λ=296nm處的共振光散射強(qiáng)度（的無私幫助和支持。ΔI）值與三聚氰胺的濃度成線性關(guān)系，線性回歸方程為ΔI=1.59c+9.70(c,10-9mol/L)，相關(guān)系數(shù)r＝0.9991，檢出限為9.1×10-9mol/L。實驗分別對4.0×10-8、8.0×10-8、1.2×10-7mol/L的三聚氰胺標(biāo)準(zhǔn)溶液分別進(jìn)行11次平行測定，相對標(biāo)準(zhǔn)偏差分別為4.54％、3.31％、4.61％，樣品加標(biāo)回收率為95.0％～97.5％。方法精密度、準(zhǔn)確度好，靈敏，操作簡便，用于食品中三聚氰胺的測定，結(jié)果滿意。
[Abstract]:Benzoic acid (BA) is a commonly used food additive. The excessive consumption of the BA affects the health of the human body and may induce cancer. The health detection of BA content is one of the important contents of food safety evaluation, and it is necessary to strengthen the health inspection of BA. Dibutyl phthalate (DBP) is a plastic plasticizer, an important environmental hormone substance, and China and the United States Environmental Protection Agency (EPA) have given DBP a priority for environmental priority control of toxic pollutants. Melamine; MM) is usually used to produce a melamine/ formaldehyde tree In human body, MM is easy to form hard-soluble salt crystallization, leading to urinary tract system calculus, bladder epithelial hyperplasia, and the like, and seriously harm human health. Kang. DBP and MM are important industrial raw materials and are the banned food additives. In recent years, DBP and MM have been illegally used as food additives, and food safety emergencies have been caused by the fact that the plasticizer has special effect on some food products. In recent years, both DBP and MM have been used as food additives. In response, the detection of DBP and MM in the food has become a high-priority food safety work in the industry and society, and the new detection methods for the establishment of these three kinds of food additives are of great significance. In this paper, based on the Fenton reaction and the resonance Rayleigh scattering spectrum, the fluorescence spectra of three kinds of toxic and harmful substances, such as BA, DBP and MM, or the new method for detecting the resonance Rayleigh scattering spectrum, are established. In the second chapter, the fluorescence spectrum of benzoic acid is established based on the Fenton reaction. In the near-neutral environment with pH = 7.6, a Fenton reagent with EDTA-Fe2 +/ H2O2 was used to capture the 路 OH radical produced by Fenton reaction with benzoic acid to form a fluorescent substance. Determination of the emission fluorescence intensity of the solution to be tested, the legal amount of the standard curve and the detection of the food at the condition of bex = 303 nm, hem = 414nm, and the pass band width of 10 nm. The RSD of three concentrations of benzoic acid at the concentrations of 7.0,10-5, 1.5,10-4 and 5.0-10-4 mol/ L was 0.40%-1.40%; s = 0.035, RSD = 3.30%. The linear regression equation is F = 98.76 c-4.12, (c,10-4 mol/ L), r = 0 .9992. Detection limit DL = 1.06-10-7 mol/ L; the lower limit of determination is 3.53-10-7 mol/ L; the linear range is determined to be 3.53-10-7-9.0-10-4 mol/ L. The recovery rate of the sample was 96.50% ~ 102.50%, RSD = 2.66%. The new method has a wide range of linear range, low detection limit and wide application; the sample processing method is simple, the operation is simple and convenient, the actual sample is accurate, accurate, and the junction is determined. The results are satisfactory. In the third chapter, the Fenton reaction produces hydroxyl radical (路 OH), DBP is hydrolyzed to produce sodium phthalate, and the reaction of the two produces the sodium phthalate of the fluorescent substance, and the indirect measurement of the sample by the fluorescence spectrometry is established. Under the optimized reaction conditions, there is a good linear relationship between the fluorescence intensity and the concentration of DBP in the range of 2.8 to 10-7-2.3 and 10-4 mol/ L. The regression equation is as follows: (F = 18.47 c-11.338 (c,10-5 mol/ L), r = 0.9970; the detection limit of the method is 8.4-10-8mol/ L, RSD of relative standard deviation is 1.4-2.6%; and the recovery rate of the sample is 96.73%- 105.68%. The method is accurate and sensitive. In the fourth chapter, the resonance Rayleigh scattering spectrum is established based on the characteristics of the resonance Rayleigh scattering spectrum. In the solution of B-R buffer solution with pH = 5.5, the melamine and barbituric acid form aggregates in a non-covalent manner in the solution of B-R buffer solution with pH = 5.5 to excite the production of melamine. Strong resonance Rayleigh scattering. The resonance light scattering intensity at a concentration of 3.03-10-8-1.60-10-7 mol/ L (Unselfish help and support. The value of "I") is linear with the concentration of melamine. The linear regression equation is" I = 1.59c + 9.70 (c,10-9 mol/ L), the correlation coefficient r = 0.9991, and the detection limit is 9.1%. 10-9 mol/ L of melamine standard solution of 4.0-10-8, 8.0-10-8, 1.2-10-7 mol/ L were tested in parallel, and the relative standard deviation was 4.54%, 3.31% and 4.61%, respectively, and the recovery of the sample was 95%. and the method has the advantages of high precision, good accuracy, sensitive and convenient operation,
【學(xué)位授予單位】：南華大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2012
【分類號】：R155.5

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