本文選題：離子色譜 + 吊白塊��； 參考：《甘肅農(nóng)業(yè)大學》2013年碩士論文

【摘要】：論文以現(xiàn)代食品安全為宗旨，以離子色譜為主要分析手段，系統(tǒng)的研究了食品中甲醛次硫酸氫鈉(俗稱吊白塊)、氫氰酸、甜蜜素的檢測方法，并對離子色譜柱、流動相等分離條件進行了優(yōu)化，得到了滿意的結果。論文主要包括以下四個方面： 1、綜述并介紹了食品安全的基本情況，詳細介紹了離子色譜儀器及應用。重點突出離子色譜對某些特殊物質(比如陰陽離子、有機酸、醇類等)檢測時的優(yōu)勢。 2、研究并建立了用離子色譜檢測食品中甲醛次硫酸氫鈉(俗稱吊白塊)的方法，對樣品前處理，色譜柱選擇，淋洗液配制等分離條件進行優(yōu)化并獲得最佳分離條件，以及對甲醛次硫酸氫鈉在不同pH溶液中的穩(wěn)定性進行了試驗研究，以滿足甲醛次硫酸氫鈉在不同基質中的檢測要求。方法檢出限為0.1mg/L；線性范圍為0.1mg/L～100mg/L；平均加標回收率分別為97.3%、90.7%、98.3%；相對標準偏差(RSD)范圍為1.4%～3.8%。適用于食品中甲醛次硫酸氫鈉的測定，該方法的靈敏度高，結果準確，方法簡單易行，為甲醛次硫酸氫鈉的實際檢測提供了理論依據(jù)。 3、研究并建立了用離子色譜-直流安培檢測食品中氫氰酸的方法，針對樣品處理，離子色譜柱的選擇，對直流安培檢測器的優(yōu)化，淋洗液的配制進行了試驗研究。檢出限為0.054mg/L；氫氰酸的線性范圍為0.136mg/L～2.72mg/L；平均加標回收率為96.8%、88.5%、100.7%；相對標準偏差(RSD)為1.6%～3.7%，可以滿足氫氰酸檢測的方法要求。 4、建立并且優(yōu)化了用離子色譜檢測食品中甜蜜素的檢測方法，并與液相色譜檢測方法做了簡單的比較，并對離子色譜檢測過程中的樣品前處理條件，色譜柱的選擇，淋洗液的配制進行了試驗研究和優(yōu)化，最終獲得最佳分離條件，方法具有分析時間短，干擾較小，適合大量樣品檢測的特點。離子色譜方法檢出限為0.5mg/L；甜蜜素的線性范圍為0.5mg/L～100mg/L；平均加標回收率分別為97.3%、97.8%、99.9%；相對標準偏差(RSD)為1%～4.1%，高效液相色譜方法檢出限為20mg/L，，甜蜜素的線性范圍為20mg/L～200mg/L；平均加標回收率分別為87.1%、92.5%、94.9%；相對標準偏差(RSD)為1.9%～6.5%，通過比較可以看出離子色譜檢測甜蜜素的方法在靈敏度等條件中具有明顯優(yōu)勢，故離子色譜檢測甜蜜素完全可以滿足對食品中甜蜜素檢測方法的要求。 綜上所述，離子色譜法檢測食品中甲醛次硫酸氫鈉、氫氰酸、甜蜜素的前處理方法簡單，能夠直接對其進行檢測，不需要對甲醛次硫酸氫鈉、甜蜜素進行繁瑣的衍生，檢測靈敏度高，明顯優(yōu)于其他檢測方法，且加標回收實驗結果滿意。
[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.

【學位授予單位】：甘肅農(nóng)業(yè)大學
【學位級別】：碩士
【學位授予年份】：2013
【分類號】：R155.5

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