本文選題：食品添加劑 + 計(jì)量�。� 參考：《中國(guó)地質(zhì)大學(xué)(北京)》2016年博士論文

【摘要】：酒類產(chǎn)品的造假和制假問(wèn)題已經(jīng)引起全社會(huì)的廣泛關(guān)注。如部分企業(yè)違規(guī)向葡萄酒中加入合成色素,用來(lái)掩蓋酒的缺陷使其成色更好,達(dá)到以次充好的目的。因此,國(guó)務(wù)院提出了針對(duì)重點(diǎn)產(chǎn)品的“打擊假冒偽劣制造,打擊盜版知識(shí)產(chǎn)權(quán)”的專項(xiàng)工作。高效液相色譜串聯(lián)技術(shù)在食品添加劑殘留領(lǐng)域研究相對(duì)很少,在上述領(lǐng)域開(kāi)展探索與研究,具備科學(xué)研究的意義與價(jià)值,本文主要酒類產(chǎn)品為基體研究對(duì)象,圍繞復(fù)雜基體(酒精度35。白酒和酒精度]5。紅酒)中多種食品添加劑殘留的計(jì)量檢測(cè)技術(shù)開(kāi)展研究。結(jié)果表明：1)研究建立了葡萄酒中安賽蜜、糖精鈉、甜蜜素、胭脂紅、莧菜紅、日落黃、檸檬黃、亮藍(lán)8種食品添加劑殘留的超高效液相色譜-串聯(lián)質(zhì)譜分析方法(UPLC-MS/MS)；采用保留時(shí)間結(jié)合2個(gè)Q1/Q3離子對(duì)進(jìn)行定性。流動(dòng)相中選擇10mmol/L的乙酸銨溶液和0.002%的三氟乙酸實(shí)現(xiàn)了8種食品添加劑的最大離子化效率。2) 8種食品添加劑在(0.03-200)u g/L范圍內(nèi)呈現(xiàn)良好的線性關(guān)系(R20.998)。方法的檢出限為(0.01～1.0)μ g/L,定量限為(0.1～1.0)μg/L。經(jīng)過(guò)方法查新與公開(kāi)發(fā)表的文獻(xiàn)報(bào)道比較,表明本論文研究的UPLC-ESI-MS/MS方法在檢出限和定量限有新穎性。本文所研究的方法不僅滿足了葡萄酒中食品添加劑殘留的快速分析需要,而且應(yīng)用于“葡萄酒中濫用食品添加劑組分測(cè)量相關(guān)計(jì)量器具量值比對(duì)”。3)用建立的方法對(duì)國(guó)內(nèi)外10種葡萄酒進(jìn)行食品添加劑殘留檢測(cè),其中2個(gè)樣品分別檢測(cè)出著色劑和甜味劑。通過(guò)建立了數(shù)學(xué)模型,確定不確定度的來(lái)源,詳細(xì)評(píng)估了不同來(lái)源分量的不確定度,最終合成得到方法的擴(kuò)展不確定度為6.0%(k=2)。4)本部分研究是建立了白酒中甜蜜素等9種甜味劑的高效液相色譜-二極管整列檢測(cè)器串聯(lián)電噴霧檢測(cè)器方法(HPLC-DAD-CAD)。通過(guò)選擇色譜柱和流動(dòng)相、優(yōu)化梯度淋洗條件和最佳柱溫,獲得了9種甜味劑的最佳色譜分離條件。其中9種甜味劑的分離度均R1.5,實(shí)現(xiàn)了基線分離,峰形對(duì)稱(不對(duì)稱度1.15-1.42),完全滿足定量分析對(duì)分離度和峰形對(duì)稱性的要求。5)本部分開(kāi)展了HPLC-DAD-CAD方法學(xué)研究,其中加標(biāo)回收率的變化范圍(88.2%-99.9%),回收率精密度變化范圍是(0.4%-3.1%)。用建立的方法對(duì)國(guó)產(chǎn)白酒進(jìn)行了甜味劑檢測(cè),其中三種白酒中檢測(cè)到甜味劑。評(píng)定了方法的不確定度,不確定度的六個(gè)主要分量(標(biāo)準(zhǔn)物質(zhì)、標(biāo)準(zhǔn)溶液配制、標(biāo)準(zhǔn)曲線擬合、樣品制備、測(cè)量重復(fù)性和回收率)分別評(píng)定,最終合成得到的方法擴(kuò)展不確定度為6.2%(k=2)。
[Abstract]:The problem of counterfeiting and counterfeiting of alcoholic products has attracted wide attention of the whole society. For example, some enterprises illegally add synthetic pigment to wine, which is used to cover up the defects of wine and make it better. Therefore, the State Council has put forward the special work of "cracking down on fake and inferior manufacturing and piracy of intellectual property rights" for key products. The research of high performance liquid chromatography series technology in the field of food additive residues is relatively few. It has scientific significance and value to carry out research in the above fields. The main liquor products in this paper are the matrix research object. Surround complex matrix (alcohol 35. 5. Liquor and alcohol] 5. The quantitative detection technique of the residue of many kinds of food additives in red wine was studied. The results showed that the results of the study were as follows: Ansai honey, sodium molasses, cyclamate, rouge, amaranth, sunset yellow, lemon yellow, amaranth, amaranth, High performance liquid Chromatography-tandem Mass Spectrometry (UPLC-MS / MS / MS) with retention time and two Q1/Q3 Ion pairs were used to determine the residues of eight bright blue additives. The 10mmol/L ammonium acetate solution and 0.002% trifluoroacetic acid were selected in the mobile phase to achieve the maximum ionization efficiency of 8 food additives. 2) the 8 food additives showed a good linear relationship in the range of 0.03-200 u / L. The detection limit of the method was 0.01 渭 g / L and the quantitative limit was 0.1 渭 g / L and 0.1 渭 g / L, respectively. The comparison between the method and the published literature shows that the UPLC-ESI-MS/MS method studied in this paper is novel in detection limit and quantitative limit. The method studied in this paper not only meets the need of rapid analysis of food additive residues in wine, And it is applied to the determination of food additive residues in 10 kinds of wine at home and abroad with the established method of "measuring the quantity ratio of relative measuring instrument in the abuse of Food Additive components in Wine". Colorants and sweeteners were detected in 2 samples. By establishing a mathematical model to determine the source of the degree of certainty, the uncertainty of the components of different sources is evaluated in detail. The extended uncertainty of the final synthesis method is 6.0kanjian2ku. 4) in this part, the method of HPLC-DAD-CADX was established for the determination of nine sweeteners such as cyclamate in liquor by high performance liquid chromatography-diode integrated detector series electrospray detector (HPLC-DAD-CADX). By selecting chromatographic column and mobile phase, optimizing gradient elution conditions and column temperature, the optimum chromatographic separation conditions of 9 sweeteners were obtained. The separation degree of 9 sweeteners is all R1.5, and the baseline separation is realized. The peak shape symmetry (asymmetric degree 1.15-1.42, which fully meets the requirements of quantitative analysis for separation degree and peak symmetry. 5) this part has carried out the HPLC-DAD-CAD methodological research. The range of recovery was 88.2-99.9, and the precision of recovery was 0.43.1. The sweeteners were detected in three kinds of liquor by the established method. The uncertainty of the method, the six main components of the uncertainty (standard material, preparation of standard solution, standard curve fitting, sample preparation, measurement repeatability and recovery) were evaluated respectively. The extended uncertainty of the method obtained by the final synthesis is 6.2%.
【學(xué)位授予單位】：中國(guó)地質(zhì)大學(xué)(北京)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2016
【分類號(hào)】：TS261.7

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