高效液相色谱-电感耦合等离子体质谱联用测定鸡肉及鸡肝中10种砷形态化合物

Determination of Ten Arsenic Species Compounds in Chicken and Chicken Liver by HPLC-ICP-MS

建立了一种有效分离检测鸡肉及鸡肝样品中洛克沙砷(ROX)、阿散酸(ASA)、硝苯胂酸(NPAA)、卡巴胂(CBS)、砷酸(AsⅤ)、亚砷酸(AsⅢ)、一甲基胂酸(MMA)、二甲基胂酸(DMA)、砷甜菜碱(As B)和砷胆碱(As C)共10种砷形态化合物的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。采用10%甲醇为提取液,碳酸铵溶液为流动相,以阴离子分析柱将样品提取液进行分离,最后进行ICP-MS测定。10种砷形态化合物在0.1~100μg/L范围内线性关系良好,相关系数(r2)均大于0.999,检出限为0.3~1.5μg/kg,定量下限为1.0~5.0μg/kg,加标回收率为81.3%~97.7%,相对标准偏差为0.1%~3.5%。该法重现性好、灵敏度高,且采用组织研磨仪机械振荡5 min即可成功提取10种砷形态化合物,与常规水浴加热振荡提取相比更加简便、高效。该法适用于鸡肉及鸡肝样品中10种砷形态化合物的同时检测,通过对实际样品的分析测定,在鸡肝样品中检出阿散酸和亚砷酸。

A method for the simultaneous determination of roxarsone （ROX ）,arsanilic acid （ASA ）,naphthalene arsenate （NPAA ）,carbarsone （CBS ）,arsenate （As Ⅴ ）,arsenite （As Ⅲ ）,methyl arsenic acid （MMA ）,dimethyl arsenic acid （DMA ）,arsenobetaine （As B ） and arsenic choline （As C ） was developed by high performance liquid chromatography and inductively coupled plasma mass spectrometry （HPLC-ICP-MS ）.The sample was extracted with 10 % methanol.The HPLC separation was performed on a Dionex IonPac AS7 anion exchange column with ammonium carbonate as mobile phase by gradient elution.Identification and quantification were achieved by ICP-MS.The linear ranges for ten arsenic species compounds were observed from 0.1 μg/L to 100 μg/L with correlation coefficients greater than 0.999.The detection limits of ten arsenic species were in the range of 0.3-1.5 μg/kg and the limits of quantitation were 1.0-5.0 μg/kg.The average recoveries for ten arsenic species spiked at three levels ranged from 81.3 % to 97.7 % with relative standard deviations of 0.1 % -3.5 % .With good reproducibility,high sensitivity,the method could extract ten arsenic species in only 5 min with organization grinding oscillation,which was much simpler and more efficient than that with conventional water bath oscillation.The method is suitable for the simultaneous determination of ten arsenic species in chicken and chicken liver.ASA and As Ⅲ were checked out in actual chicken liver samples.