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    离子色谱-电感耦合等离子体质谱法同时测定菟丝子药材中6种形态的砷

    Determination of 6 Kinds of Arsenic Species in Cuscuta by IC-ICP-MS

    • 摘要: 称取1.000 0 g经粉碎后的样品,加入0.15 mol·L-1硝酸溶液20 mL,室温放置12 h后于85℃浸提1.5 h。提取完毕,冷却至室温,以8 000 r·min-1转速离心15 min,取上层清液,经0.45 μm有机滤膜过滤后,采用AS7阴离子色谱柱(4 mm×250 mm)分离亚砷酸根、砷酸根、砷胆碱、砷甜菜碱、一甲基砷和二甲基砷,以5 mmol·L-1碳酸铵溶液和100 mmol·L-1碳酸铵溶液为流动相进行梯度洗脱,采用电感耦合等离子体质谱法测定洗脱液中的6种形态的砷。6种形态的砷的线性范围均为1.0~10.0 μg·L-1,检出限(3s)依次为0.108,0.055,0.027,0.053,0.011,0.108 μg·L-1。加标回收率在91.7%~105%之间,测定值的相对标准偏差(n=6)在1.7%~4.5%之间。

       

      Abstract: 1.000 0 g of the crushed sample was added into 20 mL of 0.15 mol·L-1 nitric acid solution, and the mixture was placed at room temperature for 12 h, then extracted at 85℃ for 1.5 h. After extraction, the mixture was cooled to room temperature and centrifuged at 8 000 r·min-1 for 15 min, and the supernatant was filtrated through 0.45 μm organic membrane. Arsenite, arsenate, arsenic, arsenobetaine, monomethyl arsenic and dimethyl arsenic were separated on an AS7 anion column (4 mm×250 mm), with 5 mmol·L-1 ammonium carbonate solution and 100 mmol·L-1 ammonium carbonate solution as the mobile phase for gradient elution, and determined by ICP-MS. The linearity range of arsenic in the six species was same 1.0-10.0 μg·L-1, and the detection limits (3s) were 0.108, 0.055, 0.027, 0.053, 0.011, 0.108 μg·L-1, respectively. Values of recovery obtained by standard addition method ranged from 91.7% to 105%. The relative standard deviations (n=6) of the measured values ranged from 1.7% to 4.5%.

       

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