尿液中6种砷形态化合物测定的高效液相色谱-电感耦合等离子体质谱法

Determination of six arsenic species in urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometr

目的建立高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)法检测尿液中亚砷酸盐、砷酸盐、一甲基砷、二甲基砷、砷胆碱和砷甜菜碱6种砷形态化合物的方法,为职业性砷中毒患者的健康评估提供依据。方法采用Hamilton PRP-X100阴离子分析柱,以磷酸铵溶液为流动相,梯度洗脱分离,进行HPLC-ICP-MS分析。结果本方法6种砷形态化合物线性关系良好,相关系数均大于0.999,方法检出限为0.46~0.57μg/L,方法定量下限为1.52~1.91μg/L,加标回收率为96.5%~106.4%,批内相对标准偏差为2.9%~6.2%,批间相对标准偏差为3.8%~8.7%。结论所建立方法灵敏度和准确度高,检测速度快,可用于职业接触人群尿液中砷形态的测定。

Objective Establishing an analysis method for the detection of six arsenic compounds trivalent arsenic,pentavalent arsenic,methyl arsenic,dimethyl arsenic,arsenical choline and arsenical betaine in urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS)and providing a theoretical basis for health assessment of arsenic poisoning patients.Methods HPLC-ICP-MS was used to detect six arsenic compounds with the hamilton PRP-X100 column and aqueous ammonium phosphate in a gradient elution as mobile phase.Results There was a good linear relationship in the selected range of six arsenic compounds evidenced by a linear correlation coefficient greater than 0.999.The detection limit of 6 arsenic compounds was 0.46~0.57μg/L,and the minimum quantitative concentration were 1.52~1.91μg/L.The recovery rates of six arsenic compounds were 96.5%~106.4%,The within-run and between-run relative standard deviation was 2.9%~6.2%and 3.8%~8.7%.Conclusion The established method with high accuracy and precision is suitable for detecting arsenic levels in urine of occupational arsenic exposure population.