高效液相色谱-原子荧光光谱 (HPLC-AFS)法测定水产动植物样品中无机砷

采用液相色谱-蒸气发生-原子荧光光谱联用技术(HPLC-HG-AFS,以下简称LC-AFS)对水产动植物样品中无机砷进行测定。藻类中以紫菜、海带、羊栖菜为研究对象,水产动物中以贝类、鱼类、虾类为研究对象,实验中研究了流动相的种类和浓度、提取剂的种类和浓度,并通过正交实验法确定了最佳提取温度、提取时间、氧化时间。在最优的实验条件下运用等度洗脱的方式测定了样品中无机砷的含量,并对方法的有效性进行了验证,结果表明,三价砷、五价砷、一甲基砷和二甲基砷在5~100μg/L范围内线性关系良好;同时对不同海产品进行加标回收实验,结果表明,各组分的加标回收率在80%~105%。平行样品测定结果的相对标准偏差在2%~6%。说明液相色谱-原子荧光光谱联用法很好地解决了水产品中砷形态测定的问题,尤其对无机砷的测定提供了非常有效的方法。方法简便、准确、设备价格低廉,完全可用于水产动植物产品中无机砷的测定。

Determination of Inorganic Arsenic in Samples of Aquatic Animals and Plants by High Performance Liquid Chromatography and Atomic Fluorescence Spectrometry (HPLC-AFS)

In this paper, high performance liquid chromatography hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS), hereinafter referred to as LC-AFS, was used for the determination of inorganic arsenicin marine products including animals and plants sample. The algae including kelp, seaweed and sargassum were used as the research object.The aquatic animals including shellfish, fish and shrimp were used as the research object.The type and concentration of mobile phase and the extraction agent were researched.The optimum extraction temperature, extraction time and oxidation time were obtained by orthogonal experiment. Under the optimal experimental conditions, the arsenic content were accurately determined using isocratic elution.And the evaluation of the method was researched,the results showed that good linear range of trivalent arsenic, pentavalent arsenic, methyl arsenic and arsenic methylation ranging from 5to 100 g/L were obtained.The experiment results indicated that the spiked recoveries of the analytes in different seafood were 80% ~ 105%, The relative standard deviationsof parallel samples were between 2% and 6%. The analysis showed that LC-AFS can be used for the detection of arsenic species in aquatic product, especially provides a very effective method for the detection of inorganic arsenic. The method using low cost equipment was simple and accurate, and it can be used entirely for the determination of inorganic arsenic in aquatic animals and plants products.