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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0.45μm有机滤膜过滤及C_(18)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0~100μg/L,相关系数均优于0.999,最低检出限为0.5μg/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。
Objective To establish a method for the determination of inorganic arsenic in aquatic products by high performance liquid chromatography-atomic fluorescence spectrometry. Methods The samples were extracted with 1% nitric acid solution and extracted with n-hexane to remove the lipid components. After filtration with 0.45μm organic membrane and C 18 column, 1 mmol / L ammonium dihydrogen phosphate solution (pH 9.0) and 20 mmol / L ammonium dihydrogen phosphate solution (pH 8.0) as a mobile phase gradient elution. Extracted liquid separated by liquid chromatography into the atomic fluorescence spectrometry, retention time qualitative, external standard method. Results The linear range of this method was 0 ~ 100μg / L, the correlation coefficient was better than 0.999, the lowest detection limit was 0.5μg / L. The spiked recoveries ranged from 87.9% to 99.3% with relative standard deviations less than 2%. Conclusion The method has the advantages of stable recovery, high sensitivity, good accuracy, less impurity interference and low detection cost. The method is suitable for the determination of inorganic arsenic in aquatic products and is convenient for application in general laboratories.