盐酸副玫瑰苯胺论文：盐酸副玫瑰苯胺 甲醛次硫酸氢钠法

盐酸副玫瑰苯胺：盐酸副玫瑰苯胺 甲醛次硫酸氢钠法 盐酸副玫瑰苯胺论文:盐酸副玫瑰苯胺 甲醛次硫酸氢钠法 【中文摘要】甲醛次硫酸氢钠(吊白块)属非食品用原料,对人体有害。目前,食品中甲醛次硫酸氢钠的测定局限在以下三种类型方法。(1)只测定甲醛来推算甲醛次硫酸氢钠的含量:有失严谨,对于只添加了甲醛的样品,经过测定后得出添加了甲醛次硫酸氢钠的结论,显然是不正确的。(2)分别测定甲醛和二氧化硫的含量,再根据二者测定结果的比值,确定是否添加有甲醛次硫酸氢钠。此方法,要做如下6个实验操作:1)按照测定甲醛的方法蒸馏样品;2)甲醛标准溶液的标定;3)测定样品中的甲醛含量;4)标定二氧化硫标准溶液;5)按照亚硫酸盐的测定方法再次处理样品;6)测定样品处理液中的二氧化硫含量。这要消耗测定人员大量的时间和精力来完成测定,而且甲醛和二氧化硫测定方法中各自的加标回收率也不一致,对添加甲醛次硫酸氢钠的量很难做出准确的判定。(3)利用离子色谱仪测定甲醛次硫酸氢根。这种方法也只能检测甲醛次硫酸氢钠形式的残留,而甲醛次硫酸氢钠遇酸或高温易分解。食品中添加甲醛次硫酸氢钠后,在其生产加工过程中,基本都有高温处理环节,甲醛次硫酸氢钠会部分或全部分解为甲醛和二氧化硫残留在食品中,这样就无法对其进行准确测定。这三类方法都存在明显的不严谨,且操作繁琐。为解决食品中甲醛次硫酸氢钠测定方法的不足,建立一种对食品广泛适用的准确、特异、灵敏、简便的检测方法,特进行本研究。本研究旨在探索一种特异、准确、灵敏、简便,广泛适用的直接测定各类食品中甲醛次硫酸氢钠的方法。 以改善以往只测定甲醛,推定出甲醛次硫酸氢钠的含量;或先测定甲醛,再测定二氧化硫,按一定的比例推算出甲醛次硫酸氢钠的含量不甚严密、繁琐的方法。试图建立一种科学地检测各类食品中甲醛次硫酸氢钠的有效的国家标准检测方法。方法含甲醛次硫酸氢钠的样品在酸性条件下通过水蒸汽蒸馏,用水进行吸收,在吸收液中,甲醛与二氧化硫生产稳定的羟甲基磺酸加成化合物,样品吸收液加入氢氧化钠,羟甲基磺酸游离出二氧化硫和甲醛,与盐酸副玫瑰苯胺反应生成一种紫红色物质,或于560 nm处用分光光度计测定其吸光度,与标准系列溶液比较定量;或用高效液相色谱法定量测定。结果用分光光度法测定时,甲醛次硫酸氢钠溶液含量在0.02,0.7 mg范围内,其响应值(吸光度)与甲醛次硫酸氢钠的含量呈强相关性,相关系数r=0.9996;检出限为0.005 mg;相对标准偏差为3.1%;回收率93.5%,107.3%。高效液相色谱法的线性范围为0.02,0.6 mg,相关系数r=0.9995;检出限为0.003 mg,若取10.00g样品,最低检出质量浓度为3 mg/kg;相对标准偏差为3.1%;加标回收率93.5%,102.2%。结论本研究的测定方法无论是分光光度法,还是高效液相色谱法,都是直接测样品中的甲醛次硫酸氢钠法,避免了过去只测定甲醛就直接推算为甲醛次硫酸氢钠可能造成的错误结果的情况,也简化了样品处理后,先测定甲醛,再测定二氧化硫,再根据二者的比例进行推算的繁琐操作过程,达到了不但可直接测定食品中添加的以甲醛次硫酸氢钠形式的残留,也可同时测定到以甲醛和二氧化硫形式存在的残留,定量准确,方法可靠,操作简便,适用于所有食品中添加甲醛次硫酸氢钠的直接测定。 【英文摘要】Sodium formaldehyde sulfoxylate is non-food raw materials, and harmful to human. At present, there are the following three types of methods for testing the Sodium formaldehyde in foods. (1) Determination of formaldehyde to project content of sodium formaldehyde sulfoxylate:this method is obviously incorrect. For the sample which only adds formaldehyde, this inference is not established. (2) Determination of formaldehyde and sulfur dioxide, respectively, then according to the ratio of two to determine whether add Sodium formaldehyde sulfoxylate. This method, do the following six experimental operation:1) distill sample according to the distillation method of determination of formaldehyde sample; 2) the calibration standard solution of formaldehyde; 3) Determination of formaldehyde content in the sample; 4) Calibration standard solution of sulfur dioxide; 5) re-treatment samples by determination of sulfite; 6) determine the content of sulfur dioxide in liquid sample. This determination consumes a lot of time and effort, and their recovery rate of two determinations of formaldehyde and sulfur dioxide are also inconsistent, it is difficult to make an accurate determination on the amount of Sodium formaldehyde sulfoxylate. (3) Determination formaldehyde hydrogen sulfate using ion chromatography. This method can only detect Sodium formaldehyde sulfoxylate residues, and Sodium formaldehyde sulfoxylate will decompose under acid or high temperature. In the production process of food, Sodium formaldehyde sulfoxylate will be part or all of the decomposition of formaldehyde and sulfur dioxide. So this method is not accurate. These three methods are not rigorous obvious, and the operation are all cumbersome. Therefore, we established an accurate, specific, sensitive and simple detection method, especially for the study.This study aimed to explore a specific, accurate, sensitive, simple, widely used method in the direct determination of sodium formaldehyde sulfoxylate in various foods. To improve those less strict, cumbersome methods, attempt to establish a scientific method, as an effective national standard testing method to test sodium formaldehyde sulfoxylate.MethodsFirst, the sample was distillated by water vapor under acidic conditions followed by the-addition of sodium hydroxide which produced sulfur dioxide and formaldehyde. Second, acting with pararosaniline hydrochloride, which generate a purple substance. Third, determining its absorbance at 560 nm, or by Quantitative comparison with the standard series solution; or directly measured by HPLC.ResultsDetermined by spectrophotometry, the content of sodium formaldehyde sulfoxylate was 0.02-0.7 mg, the response value (absorbance) and the content of sodium formaldehyde sulfoxylate was a good linearity of r=0.9996, lowest determination limit of 0.005 mg and higher recovery of 93.5%-107.3%. HPLC linear range of 0.02-0.6 mg, the correlation coefficient r= 0.9995; the detection limit was 0.003 mg, if the sample weight 10.00 g, the minimum detectable concentration was 3 mg/kg; relative standard deviations of 3.1%; the recovery rate was 93.5%-102.2%.ConclusionsIn this study, whether by the spectrophotometric determination or by high performance liquid chromatography, the sample is directly measured the sodium formaldehyde sulfoxylate. This method can avoid the wrong results caused by speculation from the content of formaldehyde. It also simplified the sample treatment, not only can detect the determination of sodium formaldehyde sulfoxylate as residue in the food, but also can detect the determination of formaldehyde and sulfur dioxide. This simple and accurate method is suitable for the direct determination of sodium formaldehyde sulfoxylate in foods. 【关键词】盐酸副玫瑰苯胺 甲醛次硫酸氢钠法(吊白块) 分光光 度法 高效液相色谱法 测定 【英文关键词】Pararosaniline Hydrochloride Sodium Formaldehyde Sulfoxylate Spectrophotometry HPLC Detection 【目录】食品中甲醛次硫酸氢钠(吊白块)的直接测定方法研究 4-6 Abstract 6-7 图和附清单 摘要 11-12 1 前言 12-15 1.1 研究背景 13-14 1.2 研究目的 14-15 2 材料与方法 15-20 2.1 技术路线 15 2.2 分光光度法 15-17 2.3 高效液相色谱法 (HPLC) 17-19 2.4 结果计算 19-20 3 实验条件优化及 结果 20-31 3.1 分光光度法部分 20-28 3.2 高效液相 色谱法部分 28-31 4 讨论 31-34 4.1 本研究的测定方 法与现有测定甲醛次硫酸氢钠的方法比较 31-33 4.2 注意事 33-34 5 结论 34-35 参考文献 35-37 综述项 37-44 1 甲醛次硫酸氢钠的性质及毒性作用 37-38 1.1 甲醛次硫酸氢钠的性质 37 1.2 甲醛次硫酸氢钠的毒性作用 37-38 2 食品中甲醛次硫酸氢钠的添加情况 38-39 2.1 食品中添加甲醛次硫酸氢钠的目的 38 2.2 食品中甲醛次硫酸 氢钠的添加状况 38-39 3 甲醛次硫酸氢钠检测的现状 39-43 3.1 只测定甲醛含量 39-40 3.2 分别测定甲醛 及二氧化硫的含量 40-42 3.3 直接检测甲醛次硫酸氢钠的状 况 42 3.4 国家标准方法概况 42-43 4 食品中甲醛次硫 酸氢钠检测方法的进展 43-44 参考文献 44-46 个人简 历 46-47 发表论文、著书及获得的科技进步奖情况 47-49 致谢 49 【索购全文找】1.3.9.9.3.8.8.4.8 1.3.8.1.1.3.7.2.1 同时提供论文写作一对一辅导和论文发表服务。 【】本文仅为中国学术文献总库合作提供，无涉版权。作者如有异议请与总库或学校联 系。