炭黑氨基柱净化HPLC-ICP-MS测定黄酒中砷形态及含量  

Simultaneous analysis of arsenic speciations and contents in rice wine by HPLC-ICP-MS

作　　者：宋伟华 胡贝贞 韩超 董文洪 

机构地区：[1]绍兴出入境检验检疫局综合技术服务中心,浙江绍兴312000 [2]温州出入境检验检疫局技术中心,浙江温州325000

出　　处：《中国酿造》2015年第3期145-149,共5页China Brewing

基　　金：浙江省公益性技术应用研究(分析测试)项目(2013C37095)

摘　　要：建立了一种同时测定黄酒中亚砷酸根、砷酸根、砷甜菜碱、一甲基砷酸和二甲基砷酸等5种砷形态的高效液相色谱-电感耦合等离子体质谱（HPLC-ICP-MS）分析方法.黄酒经炭黑氨基柱净化,体积分数为10％甲醇水溶液洗脱,采用Hamilton PRP-XIO0阴离子交换色谱柱（4.1 mm×250 mm,10 μm）,60 mmol/L硝酸铵梯度洗脱,高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析.在0.5～20.0 μg/L范围内各砷形态线性良好,相关系数R均＞0.999;加标回收率85％～92％,相对标准偏差（RSD）1.4％～5.2％;5种砷形态的定量限均为0.10μg/L,检出限均为0.03 μg/L.利用该方法对不同年份、不同企业及不同类型的黄酒进行了检测,该方法适用于黄酒中砷残留的分析检测.An analytical method for simultaneous determination of five arsenic speciations （arsenous acid radical, arsenate, arsenobetaine, MMAA, DMAA） in Chinese rice wine was developed by HPLC-ICP-MS. Samples were purified by carbon black amino column, 10% methanol aqueous solu- tion elution. The HPLC separation was performed on Hamilton PRP-XI00 negative ion analytical column （4.1 mm×250 mm, 10 μm） utilizing a gradi- ent elution program of 60 mmoFL ammonium nitrate as the mobile phase. Identification and quantification were achieved by ICP-MS. In the range of 0.5-20.0 μg/L, good linearity of 5 arsenic speciations was observed with correlation coefficients above 0.999. The adding standard recovery ranged from 85% to 92% with the relative standard deviations of 1.4%-5.2%. The quantification limits of five arsenic speciations were 0. 10 μg/L, and the detection limits were 0.03 μg/L. The proposed method was applied to the simultaneous determination of five arsenic speciations in different types of Chinese rice wine from different years and different companies, and results showed that the method was suitable for arsenic residues determination in Chinese rice wine.

关 键 词：高效液相色谱 电感耦合等离子体质谱 砷形态 黄酒 

分 类 号：O657[理学—分析化学]