电感耦合等离子体质谱法直接测定尿砷的方法研究  

Direct determination of arsenic in urine by inductively coupled plasma mass spectrometry

作　　者：徐署东 张克梅[2] 许娴[1] 常洪[2] 刘婷婷[1] 虞晨[1] 李卫东[1] Xu Shudong;Zhang Kemei;Xu Xian;Chang Hong;Liu Tingting;Yu Chen;Li Weidong(Department for Endemic and Parasitic Diseases Control and Prevention,Anhui Center for Disease Control and Prevention,Hefei 230601,China;Central Laboratory,Bengbu Center for Disease Control and Prevention,Anhui Province,Bengbu 233080,China)

机构地区：[1]安徽省疾病预防控制中心地方病与寄生虫病防治科,合肥230601 [2]安徽省蚌埠市疾病预防控制中心检验中心,233080

出　　处：《中华地方病学杂志》2020年第10期764-768,共5页Chinese Journal of Endemiology

摘　　要：目的建立尿砷含量直接快速测定的电感耦合等离子体质谱(ICP-MS)检测方法。方法新采集的人尿样品无需进行前处理,直接用纯水稀释,应用ICP-MS仪直接测定尿中总砷含量,从标准曲线的线性范围、相关系数、检出限、精密度、准确度等方面对此方法进行测试实验。结果尿砷浓度范围为0~200μg/L,仪器测定的砷与内标元素锗的粒子数之比同砷浓度呈良好线性关系,相关系数为0.9995~0.9999(n=6),尿砷最低定性检出限为0.66μg/L、定量检出限为1.94μg/L(取样量均为0.50 ml)。对5份不同砷浓度的尿液样品进行批内和批间精密度实验,相对标准偏差(RSD)范围分别为1.51%~6.84%和1.85%~5.03%。对中国疾病预防控制中心地方病控制中心尿砷考核样品进行总砷测定,检测结果在公布的公议值范围内;对砷浓度范围在3.19~89.36μg/L的4份实际尿液样品进行加标回收实验,回收率范围为99.25%~103.67%,总平均回收率为101.51%。结论应用ICP-MS法检测尿砷含量,尿液样品无需进行消解前处理,实现进样、检测和结果分析等过程的自动化,方法的灵敏度、精密度和准确度等检验参数符合生物样品检测方法研制的要求,适合尿中砷含量的快速直接测定。Objective To establish a direct and rapid method for direct determination of arsenic in urine by inductively coupled plasma mass spectrometry(ICP-MS).Methods The newly collected urine samples were diluted directly with pure water without pretreatment.The total arsenic content in urine was determined directly by ICP-MS.The method was studied from the aspects of linear range of standard curve,correlation coefficient,detection limit,precision and accuracy.Results The concentration of arsenic in urine was in the range of 0-200μg/L,the ratio of arsenic to germanium was in good linear relationship with arsenic concentration,the correlation coefficient was 0.9995-0.9999(n=6),the lowest qualitative and quantitative detection limits of arsenic in urine were 0.66 and 1.94μg/L(the sampling volume was 0.50 ml),respectively.Five urine samples with different arsenic concentrations were tested for intrabatch and inter batch precision with RSD ranging from 1.51%to 6.84%and 1.85%to 5.03%,respectively.The total arsenic of urine samples from the Center for Endemic Disease Control,Chinese Center for Disease Control and Prevention was determined with this method,and the results were within the range of the published consensus value.The recovery rate of 4 urine samples with arsenic concentration range 3.19-89.36μg/L was 99.25%-103.67%,and the total average recovery rate was 101.51%.Conclusions Application of ICP-MS method to detect arsenic content in urine,urine samples can be directly injected to realize the automation of injection,detection process and result analysis.The test parameters such as sensitivity,precision and accuracy of the method meet the requirements of the development of biological sample detection method and are suitable for rapid and direct determination of total arsenic in urine.

关 键 词：尿 砷 电感耦合等离子质谱法 直接测定 

分 类 号：R446.12[医药卫生—诊断学] O657.63[医药卫生—临床医学]