离子色谱检测食品中的吊白块、氢氰酸和甜蜜素的方法研究

发布时间：2018-04-26 04:19

本文选题：离子色谱 + 吊白块　；参考：《甘肃农业大学》2013年硕士论文

【摘要】：论文以现代食品安全为宗旨，以离子色谱为主要分析手段，系统的研究了食品中甲醛次硫酸氢钠(俗称吊白块)、氢氰酸、甜蜜素的检测方法，并对离子色谱柱、流动相等分离条件进行了优化，得到了满意的结果。论文主要包括以下四个方面： 1、综述并介绍了食品安全的基本情况，详细介绍了离子色谱仪器及应用。重点突出离子色谱对某些特殊物质(比如阴阳离子、有机酸、醇类等)检测时的优势。 2、研究并建立了用离子色谱检测食品中甲醛次硫酸氢钠(俗称吊白块)的方法，对样品前处理，色谱柱选择，淋洗液配制等分离条件进行优化并获得最佳分离条件，以及对甲醛次硫酸氢钠在不同pH溶液中的稳定性进行了试验研究，以满足甲醛次硫酸氢钠在不同基质中的检测要求。方法检出限为0.1mg/L；线性范围为0.1mg/L～100mg/L；平均加标回收率分别为97.3%、90.7%、98.3%；相对标准偏差(RSD)范围为1.4%～3.8%。适用于食品中甲醛次硫酸氢钠的测定，该方法的灵敏度高，结果准确，方法简单易行，为甲醛次硫酸氢钠的实际检测提供了理论依据。 3、研究并建立了用离子色谱-直流安培检测食品中氢氰酸的方法，针对样品处理，离子色谱柱的选择，对直流安培检测器的优化，淋洗液的配制进行了试验研究。检出限为0.054mg/L；氢氰酸的线性范围为0.136mg/L～2.72mg/L；平均加标回收率为96.8%、88.5%、100.7%；相对标准偏差(RSD)为1.6%～3.7%，可以满足氢氰酸检测的方法要求。 4、建立并且优化了用离子色谱检测食品中甜蜜素的检测方法，并与液相色谱检测方法做了简单的比较，并对离子色谱检测过程中的样品前处理条件，色谱柱的选择，淋洗液的配制进行了试验研究和优化，最终获得最佳分离条件，方法具有分析时间短，干扰较小，适合大量样品检测的特点。离子色谱方法检出限为0.5mg/L；甜蜜素的线性范围为0.5mg/L～100mg/L；平均加标回收率分别为97.3%、97.8%、99.9%；相对标准偏差(RSD)为1%～4.1%，高效液相色谱方法检出限为20mg/L，，甜蜜素的线性范围为20mg/L～200mg/L；平均加标回收率分别为87.1%、92.5%、94.9%；相对标准偏差(RSD)为1.9%～6.5%，通过比较可以看出离子色谱检测甜蜜素的方法在灵敏度等条件中具有明显优势，故离子色谱检测甜蜜素完全可以满足对食品中甜蜜素检测方法的要求。综上所述，离子色谱法检测食品中甲醛次硫酸氢钠、氢氰酸、甜蜜素的前处理方法简单，能够直接对其进行检测，不需要对甲醛次硫酸氢钠、甜蜜素进行繁琐的衍生，检测灵敏度高，明显优于其他检测方法，且加标回收实验结果满意。
[Abstract]:With the purpose of modern food safety and ion chromatography as the main analysis method, the paper systematically studies the detection methods of sodium hydrogen sulfide (commonly known as hanging white block), hydrocyanic acid and cyclamate in food, and optimizes the conditions of ion chromatography column and flow equal separation. The paper mainly includes the following four aspects. :
1, the basic situation of food safety is summarized and introduced, and the ion chromatography instrument and its application are introduced in detail. The advantages of ion chromatography for some special substances, such as Yin and Yang ion, organic acid, alcohol and so on, are highlighted.
2, a method for the determination of sodium formaldehyde sodium bisulfate (commonly known as hanging white) in food by ion chromatography is studied and established. The separation conditions such as sample pretreatment, chromatographic column selection, and leaching solution preparation are optimized and the optimum separation conditions are obtained. And the stability of sodium hydrogen sulfide in pH solution is studied to meet the application of the test. The detection limit of sodium hydrogen sulphate in different substrates is 0.1mg/L, the linear range is 0.1mg/L to 100mg/L, and the average recovery rate is 97.3%, 90.7%, 98.3%, and the range of relative standard deviation (RSD) is 1.4% ~ 3.8%. for the determination of sodium formaldehyde sulphate sodium in food. The method has high sensitivity and accurate result. The method is simple and feasible, and provides a theoretical basis for the practical detection of sodium formaldehyde bisulfite.
3, a method for the determination of hydrogen cyanic acid in food by ion chromatography DC ampere is studied and established. In the light of sample treatment and selection of ion chromatography column, the optimization of the DC ampere detector and the preparation of the leaching solution are studied. The detection limit is 0.054mg/L, the linear enclosure of hydrocyanic acid is 0.136mg/L to 2.72mg/L, and the average recovery rate is 9. 6.8%, 88.5%, 100.7%; relative standard deviation (RSD) is 1.6% - 3.7%, which can meet the requirements of the method for the detection of hydrocyanic acid.
4, the determination method of sodium cyclamate in food by ion chromatography was established and optimized, and a simple comparison with the liquid chromatography was made. The test conditions, the selection of the chromatographic column and the preparation of the leaching solution were studied and optimized in the process of ion chromatography. The optimum separation conditions were obtained, and the method had the best method. The analysis time is short and the interference is smaller. The detection limit of ion chromatography is 0.5mg/L; the linear range of cyclamate is 0.5mg/L to 100mg/L; the average recovery rate is 97.3%, 97.8%, 99.9%, the relative standard deviation (RSD) is 1% ~ 4.1%, the detection limit of high effect liquid chromatography is 20mg/L, and the linearity of cyclamate is linear The range is 20mg/L to 200mg/L, and the average recovery rate is 87.1%, 92.5%, 94.9%, and the relative standard deviation (RSD) is 1.9% ~ 6.5%. Through comparison, it can be seen that the method of ion chromatography for the determination of sodium cyclamate has obvious advantages in sensitivity and other conditions. Therefore, the determination of sweetness by ion chromatography can fully satisfy the sodium cyclamate detection side in food. The requirements of the law.
In summary, the method of ion chromatography for the determination of sodium bisulfate, hydrocyanic acid and cyclamate is simple and can be directly detected by ion chromatography. It does not need to be derived from sodium bisulfate and sodium cyclamate, and the sensitivity is high. It is obviously superior to the method of his detection, and the results of the added recovery experiment are satisfactory.

【学位授予单位】：甘肃农业大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：R155.5

【参考文献】