固相萃取光谱法测定水及食品中痕量亚硝酸盐

摘要/Abstract

摘要： 固相萃取光谱法是固相萃取与固相光谱的一种联用技术，该方法简单、快速、灵敏。样品溶液中的NO2-与对氨基苯磺酸和1-萘酚反应生成偶氮化合物，经微孔尼龙膜富集，而后不经洗脱直接测定膜光斑的漫反射-可见光谱，实现亚硝酸盐的定量分析。对pH值、样品体积、反应时间和衍生化试剂比例等反应条件，以及膜种类、富集溶液体积等固相萃取条件进行了优化，并确定分析波长为472.5 nm。在优化条件下，建立了定量分析方法。在0.002-0.030 mg/L浓度范围，吸光度y与浓度x之间呈二次函数关系，y=-268.76x2+14.55x+0.03，相关系数平方R2=0.999，检出限为1.29 μg/L。将该方法用于自来水中NO2-的检测，加标回收率在86%-125%之间，相对标准偏差在0.8%-6.6%之间；用于培根NO2-的检测，检测结果与离子色谱检测结果相符，平行实验的标准偏差在8.51%-9.99%之间。本研究为测定NO2--提供了一种具有较高的灵敏度和选择性，以及较理想的准确度和精密度的新型快检方法。

关键词: 固相萃取光谱, 固相萃取, 漫反射紫外-可见光谱, NO2-

Abstract: Solid phase extraction spectroscopy is a combination of solid phase extraction and solid phase spectroscopy, which is simple, rapid and sensitive. No2-in the sample solution reacts with p-aminobenzenesulfonic acid and 1-naphthol to form azo compound, which is enriched by microporous nylon membrane, and then the diffuse reflectance visible spectrum of membrane spot is measured directly without elution, so as to achieve the quantitative analysis of nitrite .The reaction conditions such as pH value、sample volume、reaction time and ratio of derivatization reagent, as well as solid phase extraction conditions such as membrane type and enrichment solution volume were optimized, and the analysis wavelength was determined to be 472.5 nm. Under optimized conditions, a quantitative analysis method was established. In the concentration range of 0.002-0.030mg/L, the absorbance y has a quadratic function relationship with the concentration x, y=-268.76x2+14.55x+0.03, correlation coefficient square is 0.999, and the detection limit is 1.29 μg/L. The method was applied to the detection of NO2- in tap water with the recoveries of 86%?125%, and the relative standard deviations of 0.8%?6.6%；also, the concentrations of NO2- in two types of bacon were determined. The results were comparable to those achieved by ion chromatography, and the standard deviations of parallel experiments were between 8.51% - 9.99%. This paper provides a fast method for the determination of NO2- in tap water and bacon with high sensitivity, selectivity, as well as better accuracy and precision.

Key words: Solid phase extraction spectroscopy, Solid phase extraction, Diffuse reflectance UV-Vis spectroscopy, NO2-

中图分类号:

0657.03

李超逸李龙朱莹吴婷杜一平. 固相萃取光谱法测定水及食品中痕量亚硝酸盐[J]. 食品科学, 0, (): 0-0.

Chao-Yi LI LI Long ZHU Ying WU Ting Yiping Du. Determination of trace nitrite in water and food by Solid Phase Extraction Spectrometry[J]. FOOD SCIENCE, 0, (): 0-0.

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