高效液相色谱-氢化物发生-原子荧光光谱在线联用系统分析中成药中砷化合物形态

Arsenic speciation analysis in Chinese medicine by high performance liquid chromatography-hydride generation on-line coupled with atomic fluorescence spectrometry

建立了高效液相色谱-氢化物发生-原子荧光光谱砷形态分析在线联用系统,考察了不同实验条件对4种砷形态化合物（As^Ⅲ,DMA^Ⅴ,MMA^Ⅴ和As^Ⅴ）分离分析的影响,优化了实验条件.在优化的实验条件下,采用pH 5.8的磷酸盐缓冲溶液为流动相,梯度洗脱,10 min之内4种砷形态达到基线分离.进样20μL,测定4种形态的检出限分别为：As^Ⅲ2.76 ng/mL,DMA^Ⅴ7.37 ng/mL,MMA^Ⅴ2.86 ng/mL和As^Ⅴ5.22 ng/mL,相对标准偏差RSD在2.9%～4.2%之间.该联用系统灵敏度高,准确性好,分离分析了部分市售中成药中的不同砷形态化合物.

A method based on high performance liquid chromatography-hydride generation on-line coupled with atomic fluorescence spectrometry （HPLC-HG-AFS） for arsenic speciation analysis was developed. The factors of the method including HPLC mobile phase, concentration of HCl, flow rate of HCl, concentration and flow rate of KBH4 were investigated in this paper. Under the optimum conditions, the detection limits for As^Ⅲ , DMA^Ⅴ , MMA^Ⅴ and As^Ⅴ were 2.76, 7.37, 2.86, 5.22 ng/mL, respectively. This method was applied to the analysis of arsenic species in Chinese medicine successfully.