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高效液相色谱-(紫外)氢化物发生原子荧光光谱法测定南极磷虾及其制品中6种砷形态
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作者单位
刘淑晗,张海燕,娄晓祎,孔聪,汪宇,史永富,黄宣运,沈晓盛 1.上海海洋大学食品学院2.中国水产科学研究院东海水产研究所 
基金项目:国家自然科学基金(31471672);上海市自然科学基金(17ZR1439400);中央级公益性科研院所基本科研业务费资助项目(1893-Z);上海市青年科技英才扬帆计划(18YF1429900)
中文摘要:建立了南极磷虾及其制品中6种砷形态的高效液相色谱-(紫外)氢化物发生原子荧光光谱(HPLC-(UV) HG-AFS)分析方法,对流动相浓度及pH值、泵速和负高压等条件进行了优化。在最佳实验条件下,亚砷酸(As(Ⅲ))、砷酸(As(Ⅴ))、一甲基砷酸(MMA)、二甲基砷酸(DMA)、砷甜菜碱(AsB)和砷胆碱(AsC)在5~100 μg/L范围内线性关系良好(r2>0.999 0),检出限(LOD,S/N≥3)均为0.01 mg/kg,定量下限(LOQ,S/N≥10)均为0.03 mg/kg;在0.01、0.05、0.10 mg/kg加标水平下,回收率为89.2%~108%,相对标准偏差(RSD,n=6)为3.4%~14%。采用该方法测定了南极磷虾及其制品中6种砷形态,无机砷(AsⅢ和AsⅤ)含量均低于水产品及其制品中无机砷的国家限量标准。该方法操作简单,适用范围广,结果准确可靠,可用于南极磷虾及其制品中砷的形态分析。
中文关键词:砷形态  南极磷虾  高效液相色谱-(紫外)氢化物发生原子荧光光谱法
 
Determination of Six Arsenic Speciations in Antarctic Krill and Its Products Using High Performance Liquid Chromatography-(Ultraviolet) Hydride Generation-Atomic Fluorescence Spectrometry
Abstract:A high performance liquid chromatography-(ultraviolet) hydride generation-atomic fluorescence spectrometric(HPLC-(UV)HG-AFS) method was developed for the determination of six arsenic speciations in Antarctic krill(Euphausia superba) and its products.Various instrumental conditions such as concentration and pH value of mobile phase,negative high pressure,pump speed and pretreatment conditions were optimized.Under the optimal conditions,there were good linear relationships for arsenious acid(As(Ⅲ)),arsenic acid(As(V)),monomethylarsenic acid(MMA),dimethylarsenic acid(DMA),arsenic betaine(AsB) and arsenic choline(AsC) in the range of 5-100 μg/L with correlation coefficients(r2) larger than 0.999 0.The limits of detection(LOD,S/N≥3) and quantitation(LOQ,S/N≥10) were 0.01 mg/kg and 0.03 mg/kg,respectively.Average recoveries at three spiked levels of 0.01,0.05 and 0.10 mg/kg were in the range of 89.2%-108% with relative standard deviations(RSD,n=6) of 3.4%-14%.The proposed method was successfully applied in the determination of six arsenic speciations in Antarctic krill and its products.The contents of inorganic arsenic speciations(As(Ⅲ) and As(Ⅴ)) were lower than those of the national limit standard for aquatic products and their products.The developed method is simple,wide ranging,accurate and reliable,and could be applied in the speciation analysis of arsenic in Antarctic krill and its products.
Key Words:arsenic speciation  Antarctic krill  high performance liquid chromatography-(ultraviolet) hydride generation-atomic fluorescence spectrometry
引用本文:刘淑晗,张海燕,娄晓祎,孔聪,汪宇,史永富,黄宣运,沈晓盛.高效液相色谱-(紫外)氢化物发生原子荧光光谱法测定南极磷虾及其制品中6种砷形态[J].分析测试学报,2019,(9):1085-1090.
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