高效液相色谱-荧光检测法测定婴幼儿奶粉中的亚硝酸盐  

Rapid determination of nitrite in infant milk powder by high performance liquid chromatography with fluorescence detection

作　　者：王小芳[1] 樊继彩[1] 任韧[1] WANG Xiao-fang;FAN Ji-cai;REN Ren(Hangzhou Municipal Center for Disease Control and Prevention,Hangzhou,Zhejiang 310006,China)

机构地区：[1]杭州市疾病预防控制中心,浙江杭州310006

出　　处：《中国卫生检验杂志》2021年第7期808-810,816,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立起一个简单、准确灵敏的高效液相色谱-荧光检测法,测定婴幼儿奶粉中的亚硝酸盐。方法奶粉样品经60℃水浴提取后,以亚铁氰化钾和乙酸锌溶液去除脂肪和沉淀蛋白后,上清液中的亚硝酸盐在酸性条件下和2,3二氨基萘反应生成有强荧光的物质2,3-萘三唑。反应产物经色谱柱Eclipse XDB-C_(8)(4.6 mm×150 mm,5μm)分离,流动相为水和乙腈(体积比为70∶30),流速为1.0 ml/min。采用荧光检测器进行检测,激发波长为375 nm,发射波长为415 nm。结果亚硝酸盐在0μg/L~200μg/L时具有良好的线性,相关系数为0.9999,检出限和定量限分别为0.015 mg/kg和0.050 mg/kg,回收率在94.4%~99.1%,相对标准偏差为4.11%~7.78%。结论方法操作简便、准确度好、灵敏度高,可以用于婴幼儿奶粉中亚硝酸盐的测定。Objective To establish a simple,accurate and sensitive method for the determination of nitrite in infant milk powder by high performance liquid chromatography with fluorescence detection.Methods The sample was extracted with 60℃water,after removing fat and protein with potassium hexacyanoferrate(Ⅱ)trihydrate solution and zinc acetate dihydrate solution,nitrite in the supernatant reacted with 2,3-diaminonaphthalene in acidic conditions to form a strong fluorescent substance of 2,3-naphthotriazole,which was analyzed by the high performance liquid chromatography with fluorescence detection.The analysis column was Eclipse XDB-C_(8)(4.6 mm×150 mm,5μm)column.A constant flow rate of 1.0 ml/min was employed using water-acetonitrile as mobile phase in isocratic mode(70∶30,V/V).Fluorescence was monitored with excitation at 375 nm and emission at 415 nm.Results The standard calibration curve was linear for nitrite in the concentration range of 0μg/L-200μg/L,and the correlation coefficient was 0.9999.The limit of detection was 0.015 mg/kg and the limit of quantification was 0.050 mg/kg.The recoveries of nitrite from samples spiked at three different concentrations were within 94.4%-99.1%,and the relative standard deviation of recovery results were within 4.11%-7.78%.Conclusion The proposed method is simple,accurate and sensitive,and it could be used for the determination of nitrite in infant milk powders.

关 键 词：高效液相色谱 亚硝酸盐 婴幼儿奶粉 荧光检测法 

分 类 号：O657.72[理学—分析化学]