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目的建立离子色谱-电感耦合等离子体质谱法(IC-ICP-MS)同时测定野生食用菌中砷甜菜碱(As B)、砷胆碱(As C)、二甲基砷(DMA)、一甲基砷(MMA)、亚砷酸As(Ⅲ)、砷酸As(Ⅴ)6种砷形态的方法。方法野生食用菌中砷形态用1%稀硝酸70℃超声提取1 h,离心后取上清液,残渣重复提取2次后合并上清液混匀,上清液经0.22μm滤膜过滤后通过阴离子色谱柱Dionex Ion Pac~(TM) AS7分离,2 mmol/L和100 mmol/L碳酸铵为流动相梯度洗脱,以电感耦合等离子质谱仪检测75As,外标法定量。结果 6种砷形态在0.5μg/L~50μg/L浓度线性关系良好,相关系数均为0.999 5,6种砷形态检出限为2μg/kg~8μg/kg,3个不同加标水平平均回收率为92.4%~109.1%,相对标准偏差<7%。结论该方法具有灵敏度高、准确性好的特点,可用于野生食用菌中砷形态检测分析。
Objective To establish an IC-ICP-MS method for the simultaneous determination of As B, As C, DMA, Arsenic (MMA), As (Ⅲ) arsenate, and As (Ⅴ) arsenate. Methods The arsenic speciation in wild edible fungi was extracted with 1% dilute nitric acid at 70 ℃ for 1 h. After centrifugation, the supernatant was taken and the residue was extracted twice. After the supernatant was mixed, the supernatant was filtered through 0.22 μm membrane The mobile phase was eluted with 2 mmol / L ammonium bicarbonate and 2 mmol / L ammonium bicarbonate. The analytes were determined by inductively coupled plasma mass spectrometry (75As) and external standard method. Results The linear relationships of 6 arsenic species in the range of 0.5μg / L ~ 50μg / L were good with the correlation coefficients of 0.999. The detection limits of 5,6 arsenic species ranged from 2μg / kg to 8μg / kg. The average recoveries of three different spiked levels Rates ranged from 92.4% to 109.1% with relative standard deviations <7%. Conclusion The method has the characteristics of high sensitivity and good accuracy and can be used for the determination of arsenic in wild edible fungi.