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建立了C8反相色谱短柱分离-电感耦合等离子体质谱联用技术(LCICP-M S)测定大米和紫菜中无机砷的检测方法。样品用含有2%H2O2的流动相在1000W大功率超声进行萃取(70℃,50 min),使其中的无机砷转化为五价砷,以1 mmol/L KH2PO4+1 mmol/L四丁基氢氧化铵(p H 5.5)为流动相,经C8反相色谱柱分离,电感耦合等离子体质谱仪进行定量分析。方法学验证表明:在0.5~50μg/L范围内无机砷线性良好,线性相关系数(r2)为0.9996,定量限(LOQ)为0.3μg/L,加标回收率在85.2%~109%之间,相对标准偏差(RSD,n=6)在2.1%~4.4%。方法适合于批量测定大米和紫菜样品中的无机砷。
A method was developed for the determination of inorganic arsenic in rice and seaweed by LC-RP-LC / MS coupled with LCICP-M S. The sample was extracted with high-power ultrasound at 1000W with a mobile phase containing 2% H 2 O 2 at 50 ℃ for 50 min. The inorganic arsenic was converted into pentavalent arsenic by 1 mmol / L KH2PO4 + 1 mmol / L tetrabutylammonium hydroxide (p H 5.5) as the mobile phase, separated by C8 reversed-phase column and analyzed by inductively coupled plasma mass spectrometry. The validation of the method showed that the linear range was 0.599 μg / L, the linear correlation coefficient (r2) was 0.9996, the limit of quantification (LOQ) was 0.3 μg / L and the recoveries were between 85.2% and 109% , Relative standard deviation (RSD, n = 6) ranged from 2.1% to 4.4%. The method is suitable for batch determination of inorganic arsenic in rice and seaweed samples.