改良离子色谱法测定咸鱼中亚硝酸盐的研究

Determination of nitrite in salted fish by improved ion chromatography

  • 摘要: 文章优化了现有国家标准咸鱼中亚硝酸盐的离子色谱测定方法。咸鱼样品先经硝酸银(AgNO3)除去大部分氯离子(Cl-), IC-Ag预处理柱排除剩余Cl-的干扰, 再用Ion Pac AS23(4 mm×250 mm)分析柱和Ion Pac AG23(4 mm×50 mm)保护柱, 以4.5 mmol·L-1碳酸钠(NaCO3)和0.8 mmol·L-1碳酸氢钠(NaHCO3)的溶液为淋洗液, 流速为1.0 mL·min-1, 抑制型电导检测器检测。结果显示, 用该改良方法测定不同品种咸鱼亚硝酸根离子(NO2-)的线性范围为0.01~2.00 mg·L-1, 相关系数为0.999 9, 加标回收率为83.0%~101.6%, 方法检出限为0.2 mg·kg-1。该方法前处理简便、快速, 能更加准确测定咸鱼制品的亚硝酸盐质量分数。

     

    Abstract: We determined the nitrite in salted fish by an improved ion chromatography method. The samples were first pretreated by AgNO3 solution to remove most of the Cl- and the rest of Cl- was excluded by using the Anpelclean TMIC-Ag column. Then the separation of nitrite was determined by suppressed conductivity detection on Ion Pac AS23 (4 mm×250 mm) analytical column and Ion Pac AG23 (4 mm×50 mm) guard column using 4.5 mmol·L-1 NaCO3 and 0.8 mmol·L-1 NaHCO3 as elution solvents at a flow rate of 1.0 mL·min-1. The linear range of this improved method is 0.01~2.00 mg·L-1 with correlation coefficient (R) of 0.999 9; the detection limit is 0.2 mg·kg-1and the recovery is 83.0%~101.6%. The method with simple and fast pretreatment can determine nitrite in salted fish products more accurately.

     

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