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  

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

作　　者：陈翔[1] 倪蓉[1] 路凌怡 钱杰峰[1] 刘兰侠[1] 梁卫玖 CHEN Xiang;NI Rong;LU Ling-yi;QIAN Jie-feng;LIU Lan-xia;LIANG Wei-jiu(Xuhui Center for Disease Control and Prevention,Shanghai 200237,China;不详)

机构地区：[1]上海市徐汇区疾病预防控制中心,上海200237 [2]上海市长宁区疾病预防控制中心,上海200051

出　　处：《现代预防医学》2022年第4期733-737,763,共6页Modern Preventive Medicine

摘　　要：目的建立干食用菌中砷胆碱(As C)、砷甜菜碱(As B)、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0.22μm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0.3μg/L,在0.5-100μg/L范围内,线性相关系数(r)均大于0.9995,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。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 with0.22μm 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 0.3μg/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.

关 键 词：砷形态 食用菌 微波辅助提取 高效液相色谱-电感耦合等离子体质谱法 

分 类 号：O657.63[理学—分析化学] TS219[理学—化学]