微波辅助提取-高效液相色谱-电感耦合等离子体质谱法测定干食用菌中6种砷形态

目的 建立干食用菌中砷胆碱（AsC）、砷甜菜碱（AsB）、亚砷酸根As(III)]、二甲基砷（DMA）、一甲基砷（MMA）和砷酸根As(V)]的微波辅助提取-高效液相色谱-电感耦合等离子体质谱测定方法。方法 经粉碎的干食用菌样品经1%硝酸为提取液，于100℃微波提取20 min，提取液离心、上清液经0.22 μm滤膜过滤后测定。采用Hamilton PRP - X100为分离柱，以0.1 mol/L碳酸铵(含2%甲醇）- 2%甲醇为流动相梯度洗脱。结果 方法检出限均低于0.3 μg/L，在0.5-100 μg/L范围内，线性相关系数（r）均大于0.999 5，加标回收率在97.4%～105%之间，RSD小于5%。结论 本法方法简便、快速，适用于食用菌中6种砷形态的分析。

Determination of six arsenic species in dried edible mushrooms by high performance liquid chromatography-inductively coupled plasma mass spectroscopy after microwave assisted extraction

Objective To establish a method for determination of six arsenic species including arsenocholine (AsC), arsenobetaine (AsB), arsenite As(III)], dimethyl arsenic (DMA), monomethyl arsenic (MMA) and arsenate As(V)] in dried edible mushrooms by high performance liquid chromatography-inductively coupled plasma mass spectroscopy after microwave assisted acid extraction. Methods The arsenic species in dried edible mushroom samples were extracted with 1% nitric acid by microwave at 100℃ for 20 min, then the extract was centrifuged at 9000 rpm, and finally the supernatant was filtered with 0.22 μm membrane. The filtrate was used for analysis. A Hamilton PRP-X100 anion exchange column was used for separation and the mixture of 100 mmol/L ammonium carbonate and 2% methanol was used as mobile phase for gradient elution. Results The limits of detection of the method were all less than 0.3 μg/L, and the linear ranges were within the range of 0.5-100μg/L, with the correlation coefficients greater than 0.9995. The recoveries were between 97.4% and 105%, with the relative standard deviations all less than 5%. Conclusion The method is simple and rapid, which is suitable for determination of six arsenic species in edible mushroom samples.