全自动色谱串联电感耦合等离子体质谱(LC-ICP-MS)法快速测定尿液中6种砷形态  

Rapid Determination of Six Arsenic Speciations in Urine by Fully Automated Chromatography Tandem Inductively Coupled Plasma Mass Spectrometry(LC-ICP-MS)

作　　者：姜健 徐署东 陈元元 陈宁宁 刘惠 陈曦[3] 刘柳 JIANG Jian;XU Shudong;CHEN Yuanyuan;CHEN Ningning;LIU Hui;CHEN Xi;LIU Liu(Anhui Provincial Centre for Disease Control and Prevention,Hefei,Anhui 230601,China;State Environmental Protection Key Laboratory of Environmental Health Impact Assessment of Emerging Contaminants,Shanghai Academy of Environment Sciences,Shanghai 200233,China;China CDC Key Laboratory of Environment and Population Health,National Institute of Environmental Health,Chinese Center for Disease Control and Prevention,Beijing 100050,China)

机构地区：[1]安徽省疾病预防控制中心,合肥230601 [2]上海市环境科学研究院,国家环境保护新型污染物环境健康影响评价重点实验室,上海200233 [3]中国疾病预防控制中心环境与人群健康重点实验室,中国疾病预防控制中心环境与健康相关产品安全所,北京100050

出　　处：《中国无机分析化学》2025年第4期469-475,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家自然科学基金资助项目(42077398);国家环境保护新型污染物环境健康影响评价重点实验室开放基金资助项目(SEPKLEHIAEC-202205)。

摘　　要：为准确快速测定尿液中6种砷形态,采用全自动多功能整合色谱与电感耦合等离子体质谱(ICPMS)法联用分析尿中砷甜菜碱(AsB)、亚砷酸盐[As(Ⅲ)]、二甲基砷(DMA)、砷胆碱(AsC)、一甲基砷(MMA)和砷酸盐[As(Ⅴ)] 6种砷形态。样本过0.22μm水性滤膜,20倍在线稀释,采用ICX-As35阴离子色谱柱为分析柱,0.5 mmol/L碳酸铵(pH=9.8)和80 mmol/L碳酸铵(pH=9.2)为洗脱液,梯度洗脱,在100 s左右洗脱尿中6种砷形态,建立了全自动色谱串联电感耦合等离子体质谱(IC-ICP-MS)法快速测定尿中6种砷形态的方法。6种砷形态在0~100μg/L线性关系良好,相关系数(r)均大于0.999,检出限为0.04~0.05μg/L,尿液不同浓度水平砷形态的相对标准偏差(RSD)均小于4.3%。尿液中3种不同浓度水平的加标回收率为90.0%~114%。实验结果表明,方法准确可靠、灵敏度高、分析时间短,并且不需要前处理过程,节省了时间同时减少尿中砷形态之间的转换。对我国中部某省份批量实际尿样测定过程中发现,样品中主要以DMA和As(Ⅴ)为主。To accurately and rapidly determine the urinary six arsenic speciations,fully automated multifunctional integrated chromatography coupled with inductively coupled plasma mass spectrometry(ICP-MS)was used to analyze six arsenic speciations,namely,arsenobetaine(AsB),arsenite[As(Ⅲ)],dimethylarsenic(DMA),arsenic choline(AsC),monomethylarsenic(MMA)and arsenate[As(Ⅴ)]in the urine.The samples were filtered through a 0.22μm aqueous membrane,and diluted 20 times online.The ICX-As35 anion chromatographic column was used as the analytical column,and 0.5 mmol/L ammonium carbonate(pH=9.8)and 80 mmol/L ammonium carbonate(pH=9.2)were used as the eluents for gradient elution.The six arsenic speciations were eluted in about 100 s,and a method for the rapid determination of six arsenic species in urine by fully automated chromatographic tandem inductively coupled plasma mass spectrometric(IC-ICP-MS)was established.The calibration curves showed good linearity in the range of 0-100μg/L with the correlation coefficients(r)greater than 0.999.The limits of detection(LODs)were 0.04-0.05μg/L.The relative standard deviations(RSDs)of the arsenic species at different concentration levels in urine were all less than 4.3%.The spiked recovery rate of the three different concentration levels in urine ranged from 90.0%to 114%.The results showed that the method was accurate,reliable,sensitive,short analysis time,no need for pre-treatment process,which saved time,and reduced the conversion between arsenic speciations in urine.In the determination of a large number of actual urine samples from Anhui Province,it was found that DMA and As(Ⅴ)were mainly dominant in the urine samples.

关 键 词：全自动多功能整合色谱 快速测定 砷形态 尿 

分 类 号：O657.63[理学—分析化学] O657.7[理学—化学]