食品科学 ›› 2021, Vol. 42 ›› Issue (12): 309-314.doi: 10.7506/spkx1002-6630-20191104-043

• 安全检测 • 上一篇    下一篇

固相萃取光谱法测定水及肉制品中痕量亚硝酸钠

李超逸,李龙,朱莹,吴婷,杜一平   

  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)
  • 出版日期:2021-06-25 发布日期:2021-06-29
  • 基金资助:
    上海市科委科研计划项目(17142201100)

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

LI Chaoyi, LI Long, ZHU Ying, WU Ting, DU Yiping   

  1. (Shanghai Key Laboratory of Function Materials Chemistry, East China University of Science and Technology, Shanghai 200237, China)
  • Online:2021-06-25 Published:2021-06-29

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=-268.76x2+14.55x+0.03,R2=0.999,检出限为1.29 μg/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。

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

Abstract: 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 = ?268.76x2 + 14.55x + 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.

Key words: solid phase extraction combined with spectroscopy; solid phase extraction; ultraviolet-visible diffuse reflectance spectroscopy; NaNO2; rapid determination

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