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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As3+、As5+、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 the determination of arsenic in seafood by liquid chromatography-tandem atomic fluorescence spectrometry. Methods: A suitable mobile phase (methanol + water (1 + 1) solution, hydrochloric acid solution (1.2 mol / L, 6 mol / L) / L)] to improve the extraction efficiency and resolution of As3 +, As5 +, monomethyl arsenic and dimethyl arsenic; optimize the conditions for the detection of atomic fluorescence by adjusting the lamp current, carrier gas and shielding gas flow and the concentration of oxidant and reductant , So that the fluorescence intensity of the test object to achieve the best condition. Results: The method of trivalent arsenic, pentavalent arsenic, monomethyl arsenic and dimethyl arsenic in the range of 5.0 ~ 100.0μg / L has a good linearity, the lower limit of determination of the method are 0.05 mg / kg; experiments show that The recoveries of different marine products ranged from 78% to 110% with relative standard deviations between 3.0% and 12.2%. Conclusion: The method is simple and accurate, the equipment used is cheap and can be used for the determination of four kinds of arsenic in seafood.