建立了盐藻和螺旋藻中砷形态的高效液相色谱/氢化物发生一原子荧光光谱(HPLC/HG—AFS)分析方法。优化了微藻中砷形态的提取方法、流动相浓度及PH、KBH1浓度、载流浓度、AFS参数。优化后砷形态的提取效率范围为97.3%~99.1%,在优化后的实验条件下,As(Ⅲ)、二甲基砷酸(DMA)、一甲基砷酸(MMA)和As(V)的线性相关系数分别为0.9999、0.9996、0.9997和o.9994,检出限分别为0.19、0.40、0.34、0.52μg/L,盐藻的砷加标回收率为91.5%~100.8%,螺旋藻的砷加标回收率为95.6%~104.59/6。研究结果表明,该方法检测快速(10min),且测得微藻中的砷形态数据准确、可靠。
A method using high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry(HPLC/HG-AFS) to determine arsenic speciation in Dunaliella tertiolecta and Spirulina platensis has been developed. Various operating parameters including extraction procedures of arsenic species in microalgae, the concentration of mobile phase and pH, potassium borohydride solution, carrier solution and the AFS conditions were optimized. Under the optimal experimental conditions, extraction efficiency in the range of 97. 3%-99. 1%, and the linear correlation coefficients of 0. 9999, 0. 9996,0. 9997 and 0. 9994 for As( Ⅲ ), dimethyl-arsonic acid(DMA), monomethyl-arsonic acid(MMA) and As(V ),and the limits of detection of 0.19,0. 40,0. 34 and 0.52 μg/L were obtained, respectively. The recoveries of arsenic species for spiked Dunaliella tertiolecta were about 91.5%-100.8%, and the recoveries of arsenic species for spiked Spirulina platensis were about 95. 6%. 104.5%. The results indicated that HPLC-HG-AFS was a reliable method for fast determination(10 min) of arsenic species in microalgae.