摘要
该研究旨在采用HPLC-ICP-MS建立同时测定砷甜菜碱(As B)、砷胆碱(As C)、二甲基砷(DMA)、亚砷酸根[As(Ⅲ)]、一甲基砷(MMA)和砷酸根[As(Ⅴ)]6种形态砷的检测方法。采用Dioncx Ion Pac^TMAS7阴离子交换柱(4 mm×250mm),以100 mmol·L^-1碳酸铵(A)-1.5 mmol·L^-1磷酸氢二铵(B)为流动相,进行梯度洗脱,流速1 m L·min^-1,进样量10μL。方法学结果显示,As B,As C,DMA,As(Ⅲ),MMA和As(Ⅴ)质量浓度在10~500μg·L^-1线性关系良好(R2>0.999);平均加样回收率(n=6)分别为105.7%,100.5%,102.9%,105.7%,100.2%,92.69%,RSD分别为0.50%,2.4%,0.93%,1.3%,0.89%,1.5%;此方法精密度与重复性均良好。在所建立的色谱条件下,6种形态砷均得到良好的分离;经方法学验证和实际样品测定,该方法可用于砷形态价态化合物的含量测定。
This study aims to establish a method for the determination of As B,As C,DMA,As(Ⅲ),MMA and As(Ⅴ)by using HPLC-ICP-MS.A Dioncx Ion Pac^TMAS7(4 mm×250 mm)column was used for the HPLC-ICP-MS method.The mobile phase was 100 mmol·L^-1 ammonium carbonate-1.5 mmol·L^-1 ammonium dibasic phosphate(gradient elution)at a flow rate of 1 m L·min^-1.The injection volume was 10μL.The linear relationships of As B,As C,DMA,As(Ⅲ),MMA,As(Ⅴ)were good with the concentration of10-500μg·L^-1.The average recovery rates(n=6)were 105.7%,100.5%,102.9%,105.7%,100.2%,92.69%.The RSD were0.50%,2.4%,0.93%,1.3%,0.89%,1.5%.The precision and repeatability of this method were good.In this study,six forms of arsenic were separated effectively by this method.With methodological validation and sample determination,this method can be used to determine the morphological valence of arsenic in content determination.
作者
李耀磊
王莹
王赵
金红宇
马双成
LI Yao-lei;WANG Ying;WANG Zhao;JIN Hong-yu;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2019年第24期5441-5445,共5页
China Journal of Chinese Materia Medica
基金
国家“重大新药创制”科技重大专项(2014ZX09304307-002).
