复杂基体中多种食品添加剂计计量检测技术研究

发布时间：2018-06-07 13:36

本文选题：食品添加剂 + 计量　；参考：《中国地质大学(北京)》2016年博士论文

【摘要】：酒类产品的造假和制假问题已经引起全社会的广泛关注。如部分企业违规向葡萄酒中加入合成色素,用来掩盖酒的缺陷使其成色更好,达到以次充好的目的。因此,国务院提出了针对重点产品的“打击假冒伪劣制造,打击盗版知识产权”的专项工作。高效液相色谱串联技术在食品添加剂残留领域研究相对很少,在上述领域开展探索与研究,具备科学研究的意义与价值,本文主要酒类产品为基体研究对象,围绕复杂基体(酒精度35。白酒和酒精度]5。红酒)中多种食品添加剂残留的计量检测技术开展研究。结果表明：1)研究建立了葡萄酒中安赛蜜、糖精钠、甜蜜素、胭脂红、苋菜红、日落黄、柠檬黄、亮蓝8种食品添加剂残留的超高效液相色谱-串联质谱分析方法(UPLC-MS/MS)；采用保留时间结合2个Q1/Q3离子对进行定性。流动相中选择10mmol/L的乙酸铵溶液和0.002%的三氟乙酸实现了8种食品添加剂的最大离子化效率。2) 8种食品添加剂在(0.03-200)u g/L范围内呈现良好的线性关系(R20.998)。方法的检出限为(0.01～1.0)μ g/L,定量限为(0.1～1.0)μg/L。经过方法查新与公开发表的文献报道比较,表明本论文研究的UPLC-ESI-MS/MS方法在检出限和定量限有新颖性。本文所研究的方法不仅满足了葡萄酒中食品添加剂残留的快速分析需要,而且应用于“葡萄酒中滥用食品添加剂组分测量相关计量器具量值比对”。3)用建立的方法对国内外10种葡萄酒进行食品添加剂残留检测,其中2个样品分别检测出着色剂和甜味剂。通过建立了数学模型,确定不确定度的来源,详细评估了不同来源分量的不确定度,最终合成得到方法的扩展不确定度为6.0%(k=2)。4)本部分研究是建立了白酒中甜蜜素等9种甜味剂的高效液相色谱-二极管整列检测器串联电喷雾检测器方法(HPLC-DAD-CAD)。通过选择色谱柱和流动相、优化梯度淋洗条件和最佳柱温,获得了9种甜味剂的最佳色谱分离条件。其中9种甜味剂的分离度均R1.5,实现了基线分离,峰形对称(不对称度1.15-1.42),完全满足定量分析对分离度和峰形对称性的要求。5)本部分开展了HPLC-DAD-CAD方法学研究,其中加标回收率的变化范围(88.2%-99.9%),回收率精密度变化范围是(0.4%-3.1%)。用建立的方法对国产白酒进行了甜味剂检测,其中三种白酒中检测到甜味剂。评定了方法的不确定度,不确定度的六个主要分量(标准物质、标准溶液配制、标准曲线拟合、样品制备、测量重复性和回收率)分别评定,最终合成得到的方法扩展不确定度为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%.
【学位授予单位】：中国地质大学(北京)
【学位级别】：博士
【学位授予年份】：2016
【分类号】：TS261.7

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