机构地区: 深圳出入境检验检疫局
出 处: 《中国卫生检验杂志》 2009年第9期1955-1958,1993,共5页
摘 要: 目的:建立液相色谱串联原子荧光光谱仪检测海产品中不同形态的砷的测定方法。方法:选择合适的提取液(甲醇+水(1+1)溶液、盐酸溶液(1.2 mol/L,6 mol/L))和合适的流动相[pH6.0的磷酸氢二铵溶液(15 mmol/L)〗来提高As^3+、As^5+、一甲基砷和二甲基砷的提取效率和分离度;通过调整灯电流、载气和屏蔽气流量以及氧化剂和还原剂的浓度,优化原子荧光检测条件,使待测物的荧光强度达到最佳状态。结果:本方法的三价砷、五价砷、一甲基砷和二甲基砷在5.0-100.0μg/L范围内有良好的线性,方法的测定低限均为0.05 mg/kg;实验表明方法对不同海产品的回收率在78%-110%之间,相对标准偏差在3.0%-12.2%之间。结论:该方法简便、准确,所使用的设备价格低廉,可用于海产品中4种砷形态的测定。 Objective: To establish a method for determination of four different arsenic species in marine products by high performance liquid chromatography- atom flurecent spectrpmetry. Methods:50%, 10% hydrochloric acid solution and 50% methanol solution were used to increase extraction efficiency, and the optimized mobile phase was 15 mmol/L diammonium phosphate (pH6. 0). The lamp current, velocity of cartier gas, velocity of auxiliary gas, concentrations of oxidant and reducing agent were also optimized. Results :The linear ranges for inorganic arsenic, monomethylarsonic acid and dimethylarsonic acid were all from 5.0 to 100. 0 μg/L. The detection limits of As^3+ , As^5+ , monomethylarsonic acid and dimethylarsonic acid were 0.05 mg/kg. The recoveries of the method were 78 % - 110% (n = 6), and the relative standard deviations were 3.0% - 12. 2 %. Conclusion:This method is simple and convenient, and can be used to analyze four arsenic species in marine products.