摘要
目的建立高效液相色谱(HPLC)-原子荧光光谱(AFS)测定人血液中4种形态砷化合物。方法优化HPLC-AFS联用技术测定急性砷中毒患者血液中亚砷酸盐[As(III)]、二甲基砷酸(DMA)、一甲基砷酸(MMA)和砷酸盐[As(V)]4种形态砷化合物时色谱分离条件、样品预处理条件以及原子荧光检测参数,测试了批内、批间精密度、加标回收试验等方法学性能指标。结果该方法测定As(III)的线性范围为2.63~100.00μg/L,相关系数为0.9999,检出限为2.63μg/L;DMA的线性范围为3.21~100.00μg/L,相关系数为0.9992,检出限为3.21μg/L;MMA的线性范围为3.41~100.00μg/L,相关系数为0.9998,检出限为3.41μg/L;As(V)的线性范围为3.90~100.00μg/L,相关系数为0.9996,检出限为3.90μg/L。样品加标回收率为91.3%~99.8%,相对标准偏差(RSD)为2.39%~4.05%,批内、批间精密度分别为1.99%~4.59%、2.72%~4.53%。结论该方法检出限低、线性范围宽、精密度好、灵敏度高,适用于急性砷中毒患者血液中形态砷化合物的测定。
Objective To establish a method for determination of arsenic species in blood with high performance liquid chromatography-atomic fluorescence spectrometry(HPLC-AFS).Methods The effect of mobile phase about chromatography separation and sample pretreatment conditions and atomic fluorescence spectrometry detection parameters has been optimized to reliably measure the following four kinds of species arsenic compound including arsenic[As(III)]、dimethylarsinic acid(DMA)、monomethylarsonic acid(MMA)and arsenate[As(V)]in acute intoxication human blood.The method of technical standard about within-run,between-run and recoveries of standard were optimized.Results The method showed As(III)linear relationship was 2.63-100.00μg/L,The detection limit was 2.63μg/L.The relative coefficient(r)was 0.9999;DMA linear relationship was 3.21-100.00μg/L,The detection limit was 3.21μg/L.The r was 0.9992;MMA linear relationship was 3.41-100.00μg/L,The detection limit was 3.41μg/L.The r was 0.9998;As(V)linear relationship was 3.90-100.00μg/L,The detection limit was 3.90μg/L.The r was 0.9996.The average recovery of four species arsenic in tested samples ranged from 91.3%-99.8%with the relative standard deviation(RSD)from 2.39%to 4.05%.The within-run and between-run relative standard deviations(RSD)of repetitive measurement at 10.00,40.00,80.00μg/L concentration levels were 1.99%-4.59%and 2.72%-4.53%.Conclusion This method is low detection limit,good accurate and high sensitivity,proposed method had been applied to the analysis of arsenic species in blood samples those who acute intoxication or poisoning diagnosis.
作者
周乐舟
杨露
付胜
Zhou Lezhou;Yang Lu;Fu Sheng
出处
《中华劳动卫生职业病杂志》
CAS
CSCD
北大核心
2019年第12期928-931,共4页
Chinese Journal of Industrial Hygiene and Occupational Diseases
基金
湖南省自然科学基金(2018JJ6021)。
关键词
色谱法
液相
光谱法
荧光
形态砷
血液
急性中毒
Chromatography,liquid
Spectrometry,fluorescence
Arsenic species
Blood
Acute intoxication
