摘要
目的:利用过氧化氢氧化与阀切换离子色谱法测定食盐中亚硝酸盐含量。方法:利用氧化剂(过氧化氢)将食盐样品溶液中的NO_(2)^(-)氧化为NO_(3)^(-),再通过阀切换,洗脱大部分Cl^(-)和Br^(-),收集氧化生成的NO_(3)^(-)于定量环中,定量环中的NO_(3)^(-)经氢氧化钾淋洗液进入AS11-HC保护柱(50 mm×4 mm)和分析柱(250 mm×4 mm)进行分离,再进行电导检测,通过检测NO_(3)^(-)的含量间接得到NO_(2)^(-)的含量。结果:在0.01~1.00 mg·L^(-1)的线性范围内,r=0.9999,RSD(n=7)为2.3%,检测限为8.57×10^(-4)mg·L^(-1),回收率为85.2%~111.0%。22个样品中5个样品未检出NO_(2)^(-),其他样品介于6.94~88.70μg·g^(-1)。结论:该实验方法准确、灵敏,可应用于食盐中亚硝酸盐的检测。
Objective: To develop a new ion chromatographic(IC-CD) method for the determination of nitrite in salt by using H_(2)O_(2) oxidation couple with valve-switching. Methods: NO_(2)^(-) in samples was first oxidized to NO_(3)^(-)by H_(2)O_(2),and then removed most Cl^(-) and Br^(-) through valve-switching. After that NO_(3)^(-) was collected in the sample loop and finally was injected into ion chromatography separation and detection. The operation was performed on Ion AS11-HC guard column(50 mm×4 mm) and analytical column(250 mm×4 mm),and KOH was as gradient elution. The content of NO_(2)^(-) was calculated indirectly by detection of NO_(3)^(-) in the sample after oxidation. Results: The calibration plots for NO_(2)^(-) were linear in the range from 0.01 to 1.00 mg·L^(-1) with good correlation(r=0.999 9). The relative standard deviation(RSD) was 2.3%(n=7), the limit of detection(LOD) was 8.57×10^(-4) mg·L^(-1). The recovery of nitrite in real samples were between 85.2% and 111.0%.The content of NO_(2)^(-) in 17 samples was 6.94-88.70 mg·L^(-1), and the other 5 samples were not detected. Conclusion: The method is accurate and sensitive, and could be applied to the determination of nitrite in salt.
作者
唐嘉怡
郑杨杨
黄雪婷
Nesterenko Pavel N
叶明立
陈梅兰
TANG Jia-yi;ZHENG Yang-yang;HUANG Xue-ting;Nesterenko Pavel N;YE Ming-li;CHEN Mei-lan(College of Biological and Environmental Engineering,Zhejiang Shuren University,Hangzhou 310015,China;Chemistry Department,Physical Chemistry Division,Lomonosov Moscow State University,Moscow 119991,Russia)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2023年第12期2105-2112,共8页
Chinese Journal of Pharmaceutical Analysis
