微波消解-氢化物原子荧光光谱法测定大米中的总砷

Determination of total arsenic in rice by microwave digestion hydride generation atomic fluorescence spectrometry

针对《食品中总砷及无机砷的测定》GB 5009.11—2014对食品中总砷的测定方法进行了改进。根据国家标准GB 5009.11—2014总砷的测定中氢化物原子荧光光谱法,分别采用微波消解与湿法消解对质控样品和试样样品处理后进行总砷含量的测定。结果表明:总砷在0~10.0μg/L线性范围的相关系数为0.9998,微波消解法结果相对标准偏差为0.64%~1.60%,加标回收率为94%~106%;湿法消解结果相对标准偏差为2.80%~4.94%,加标回收率为84%~86%。相比GB 5009.11—2014总砷第二法中试样消解的湿法消解法,微波消解法具有仪器自动化程序高,前处理操作简单快速安全;酸消耗量较少、种类单一,试剂污染小;可进行大批量处理,检测结果准确度高、平行样品间精密度较好、回收率高的优点。

According to the determination of total arsenic and inorganic arsenic in food GB 5009.11-2014,the determination method of total arsenic in food was improved.According to the national standard GB 5009.11-2014,hydride generation atomic fluorescence spectrometry was used to determine the content of total arsenic in quality control samples and samples after treatment by microwave digestion and wet digestion.The results showed that the correlation coefficient of total arsenic in the linear range of 0~10.0μg/L was 0.9998,the relative standard deviation of microwave digestion method was 0.64%~1.60%,and the recovery was 94%~106%;the relative standard deviation of wet digestion method was 2.80%~4.94%,and the recovery was 84%~86%.Compared with the wet digestion method of sample digestion in the second method of total arsenic in GB 5009.11-2014,the microwave digestion method has the advantages of high instrument automation program,simple,fast and safe pretreatment operation,less acid consumption,single type,less reagent pollutions,large batch processing,high accuracy of detection results,good precision between parallel samples and high recovery rate.