高效液相色谱-原子荧光联用技术测定 水产品中无机砷

Determination of inorganic arsenic in aquatic products by atomic fluorescence spectrometry coupled with high performance liquid chromatography

中文关键词:  无机砷  高效液相色谱法  原子荧光光谱法

英文关键词:inorganic arsenic  high performance liquid chromatography  atomic fluorescence spectrometry

中文摘要:

      目的 建立一种高效液相色谱-原子荧光联用技术测定水产品中无机砷的测定方法。方法 样品经1%的硝酸溶液提取, 正己烷萃取去除脂质成分, 并用0.45 μm有机滤膜过滤及C18小柱净化后, 采用1 mmol/L磷酸二氢铵溶液(pH 9.0)和20 mmol/L的磷酸二氢铵溶液(pH 8.0)作为流动相进行梯度洗脱。提取液经液相色谱分离后进入原子荧光光谱仪测定, 以保留时间定性, 外标法定量。结果 该方法的线性范围为0~100 μg/L, 相关系数均优于0.999, 最低检出限为0.5 μg/L。加标回收率在87.9%~99.3%范围内, 相对标准偏差均小于2%。结论 该方法回收率稳定、灵敏度高、准确度好、杂质干扰少、检测成本低, 适用于水产品中无机砷的测定, 便于在普通实验室应用。

英文摘要:

      Objective To establish a method for the determination of inorganic arsenic in aquatic products by high performance liquid chromatography-atomic fluorescence spectrophotometry (HPLC-AFS). Methods Samples were extracted with 1% nitric acid solution, and removed lipids with n-hexane. The extracts were filtrated by 0.45 μm organic membranes and purified with C18 column. After using 1 mmol/L ammonium dihydrogen phosphate solution (pH 9.0) and 20 mmol/L ammonium dihydrogen phosphate solution (pH 8.0) as mobile phase, the extracts which were separated by liquid chromatography were detected by atomic fluorescence spectrometry, using retention time for qualitative assay and external reference method for quantitative assay. Results The linear ranges of arsenite (AsIII) and arsenate (AsV) were 0~100 μg/L. The correlation coefficients were all above 0.999. The limits of detection were 0.5 μg/L and the recoveries of standard addition were 87.9%~99.3%, respectively. The relative standard deviations (RSD) of this precision were less than 2%. Conclusion The established method has stable recoveries, high sensitivity, specificity and low detection cost, which can meet the determination requirements of inorganic arsenic in aquatic products and facilitate to application in general laboratories.