固相萃取光谱法测定水及肉制品中痕量亚硝酸钠  

Spectroscopic Determination of Trace Nitrite in Water and Meat Following Solid Phase Extraction

作　　者：李超逸 李龙[1] 朱莹 吴婷[1] 杜一平[1] LI Chaoyi;LI Long;ZHU Ying;WU Ting;DU Yiping(Shanghai Key Laboratory of Function Materials Chemistry,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学上海市功能性材料化学重点实验室,上海200237

出　　处：《食品科学》2021年第12期309-314,共6页Food Science

基　　金：上海市科委科研计划项目(17142201100)。

摘　　要：采用固相萃取光谱法对亚硝酸钠进行定量分析。首先确定分析波长为472.5 nm,随后优化衍生化反应的条件:pH 4.74、衍生化时间15 min、衍生化试剂亚硝酸钠-对氨基苯磺酸-1-萘酚物质的量比1∶3∶3。富集条件:富集膜种类为尼龙膜,过膜体积为10 mL。在0.002~0.030 mg/L质量浓度范围,吸光度y与质量浓度x之间呈二次函数关系,y=-268.76x^(2)+14.55x+0.03,R^(2)=0.999,检出限为1.29μg/L。将该方法用于自来水中亚硝酸钠的检测,加标回收率在91.3%~114.0%之间,相对标准偏差在4.21%~7.90%之间;用于培根亚硝酸钠的检测,检测结果与离子色谱检测结果相符,平行实验的相对标准偏差分别为8.51%、9.98%。本研究为测定亚硝酸钠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速检测方法。A spectroscopic method was used for the quantitative analysis of sodium nitrite after solid phase extraction. The analytical wavelength was set at 472.5 nm, and the derivatization conditions were optimized as follows: pH 4.74, derivatization time 15 min, and derivatization reagent composition sodium nitrite:p-aminobenzenesulfonic acid:1-naphthol molar ratio of 1:3:3. Enrichment was accomplished using a nylon membrane with a loading volume of 10 mL. In the concentration range of 0.002–0.030 mg/L, the absorbance(y) had a quadratic relationship with nitrite concentration(x), expressed as y =-268.76 x2 + 14.55 x + 0.03, with a correlation coefficient(R2) of 0.999, and the limit of detection(LOD) of the presented method was 1.29 μg/L. The method was applied to the detection of NaNO2 in tap water with spiked recoveries of 91.3%–114.0%, and relative standard deviations(RSDs) of 4.21%–7.90%. The results of this method for sodium nitrite in bacon agreed with those of ion chromatography, with standard deviations of 8.51% and 9.98% in parallel experiments on American-style and Shuanghui-branded bacons, respectively. This study has provided a rapid, sensitive, accurate and precise method for the determination of NaNO2 with high selectivity.

关 键 词：固相萃取光谱 固相萃取 漫反射紫外-可见光谱 亚硝酸钠 快速检测 

分 类 号：O657.03[理学—分析化学]