Citation: LIU Cheng-Xin, XIAO Zhi-Ming, JIA Zheng, TIAN Jing, LIU Xiao-Lu, FAN Xia. Quantitative Determination of Arsenic Species in Feed Using Liquid Chromatography-Hydride Generation Atomic Fluorescence Spectrometry. Chinese Journal of Analytical Chemistry, 2018, 46(4): 537-542. doi: 10.11895/j.issn.0253-3820.171228 [复制]
Quantitative Determination of Arsenic Species in Feed Using Liquid Chromatography-Hydride Generation Atomic Fluorescence Spectrometry
建立了饲料中亚砷酸盐（As3+）、砷酸盐（As5+）、一甲基砷酸（MMA）、二甲基砷酸（DMA）、对氨基苯胂酸（p-ASA）、羟基苯胂酸（4-OH）和洛克沙胂（ROX）共7种不同形态砷的高效液相色谱-氢化物发生原子荧光光谱（HPLC-HG-AFS）分析方法。饲料样品采用甲醇-水（1:1，V/V）溶液提取，15 mmol/L（NH4）2HPO4和10 mmol/L邻苯二甲酸氢钾为流动相，经PRP-X100阴离子交换色谱柱分离后，由HG-AFS测定。结果表明，7种砷形态标准曲线的线性关系良好（R2≥0.9964），方法检出限为5~30 μg/kg，平均回收率为76.3%~108.1%，日内相对标准偏差≤7.7%，日间相对标准偏差≤17.4%。本方法灵敏度高、前处理简单、运行费用低廉，适用于饲料产品中砷的形态分析。
A sensitive and rapid method using liquid chromatography-hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS) was developed for the simultaneous determination of seven arsenic species As3+, As5+, MMA, DMA, p-ASA, 4-OH and ROX in feeds. The isolation of the analytes from feed samples was accomplished using methanol water (1:1, V/V). The target compounds were separated on a PRP-X100 anion exchange column and then analyzed by HG-AFS. The mobile phase was 15 mmol/L (NH4)2HPO4 and 10 mmol/L potassium acid phthalate. Good linearity was obtained for all of the seven arsenic species, with linear coefficients higher than 0.9964. The LODs of the seven arsenic species were between 5 and 30 μg/kg. Average recoveries for the seven analytes were in the ranges of 76.3%-108.1%, with intra-and inter-day repeatability lower than 7.7% and 17.4%, respectively. This validated method was successively applied to the determination of arsenic species in feed. This method was sensitive, simple, cheap and low operation cost, and could be used for the determination of the arsenicspecies in feeds.