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目的建立不同方法测定大米和以大米为原料的食品中无机砷的含量,并对结果进行比较。方法用0.15 mol/L硝酸或0.3 mol/L三氟乙酸作为提取液,95℃下热辅助提取2 h、75℃下超声提取2 h或90℃下微波辅助提取1 h,提取物经阴离子交换柱X-100(250 mm×4.1 mm,10μm)分离,电感耦合等离子体-质谱(ICP-MS)和氢化物发生-原子荧光光谱(HG-AFS)分别测定。结果两种方法测定无机砷含量,加标回收率分别在94.8%～111.7%、91.9%～96.0%之间,相对标准偏差均小于5.8%,应用这两种方法对质控样品米粉SRM 1568a和大米样品进行测定,结果协同性良好。结论两种方法均可简单、准确、快速的测定大米中的无机砷,结果比较差异无统计学意义。
Objective To establish different methods to determine the contents of inorganic arsenic in rice and rice-based foods, and compare the results. Methods The samples were extracted with 0.15 mol / L nitric acid or 0.3 mol / L trifluoroacetic acid for 2 h by heat-assisted extraction at 95 ° C, 2 h by ultrasonic extraction at 75 ° C or 1 h by microwave-assisted extraction at 90 ° C. The column X-100 (250 mm × 4.1 mm, 10 μm) separation was used for the determination of Hb-AFS by inductively coupled plasma-mass spectrometry (ICP-MS) and hydride generation- atomic fluorescence spectrometry (HG-AFS). Results The two methods were used to determine the content of inorganic arsenic. The recoveries of the two methods were 94.8% ~ 111.7% and 91.9% ~ 96.0%, respectively. The relative standard deviations were both less than 5.8% Rice samples were measured, the results of good coordination. Conclusion Both methods can be simple, accurate and rapid determination of inorganic arsenic in rice, the results showed no significant difference.