摘要
建立了液相色谱-原子荧光光谱(LC-AFS)法测定大米中无机砷的方法。将样品中的无机砷经稀硝酸提取后,以液相色谱进行分离。分离后的目标物在酸性环境下与KBH4反应,生成气态砷化合物,以原子荧光光谱仪进行测定。实验结果表明,在0~100.0 ng/m L的浓度范围内,大米中无机砷含量与响应值呈现良好的线性关系(R≥0.999),无机砷的回收率分别为97.9%~101.0%[As(III)]和99.2%~102.1%[As(V)],重复性测定结果为0.81%~2.23%[As(III)]和1.34%~2.15%[As(V)],无机砷的方法检出限为0.007 2 mg/kg[As(III)]和0.022 9 mg/kg[As(V)],定量限为0.017 9 mg/kg[As(III)]和0.057 2 mg/kg[As(V)]。该方法检测准确度高,具有良好的精密度,适用于大米中无机砷的检测。
The determination method of inorganic arsenic in rice by using the liquid chromatography atomic fluorescence spectrometry(LCAFS)is developed.The inorganic arsenic in rice samples is extracted by using dilute nitric acid,and is separated by liquid chromatography.The target object after separation reacts with KBH4in acidic environment,and generates gaseous arsenic compounds,which are determined by atomic fluorescence spectrometer.The research results show that in the concentration range of0~100.0ng/mL,the inorganic arsenic content in rice presents a good linear relationship with the response value(R≥0.999),the recoveries of inorganic arsenic are97.9%~101.0%[As(III)]and99.2%~102.1%[As(V)]respectively,repeatability test results are0.81%~2.23%[As(III)]and1.34%~2.15%[As(V)],the detection limits of inorganic arsenic are0.0072mg/kg[As(III)]and0.0229mg/kg[As(V)];the quantitative limits are0.0179mg/kg[As(III)]and0.0572mg/kg[As(V)].The method has high detection accuracy,good precision,and is suitable for the determination of inorganic arsenic in rice.
作者
顾锦明
周瑾
Gu Jinming;Zhou Jin(Pudong New Area Station of Measurement and Quality Inspection,Shanghai)
出处
《上海计量测试》
2017年第2期9-12,共4页
Shanghai Measurement and Testing
