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液相色谱-氢化物发生原子荧光光谱测定鸡肉中 4种形态砷化合物
陈玎玎,葛高飞
0
(安徽农业大学生物技术中心,合肥 230036)
摘要:
建立了鸡肉中三价砷(As(Ⅲ))、一甲基砷(MMA)、二甲基砷(DMA)和五价砷(As(Ⅴ))的4种砷形态的高效液相色谱-氢化物发生原子荧光光谱(HPLC-HG-AFS)分析方法。样品采用0.15 mol·L-1稀硝酸+超声波进行提取,以5 mmol·L-1 Na2HPO4和45 mmol·L-1 KH2PO4缓冲液(pH5.92)为流动相,经PRP-X100 阴离子交换色谱柱分离后,原子荧光光谱测定。结果表明,4种形态的砷在8 min内实现良好分离,标准曲线的线性关系良好(r≥0.999),方法检出限为1.0~3.0 μg·L-1,6次平行测定的相对标准偏差(RSD)为2.0%~6.2%(100 μg·L-1)。鸡肉样品的加标回收率为82.1%~101%。
关键词:  砷形态  液相色谱  氢化物发生原子荧光光谱  鸡肉
DOI:10.13610/j.cnki.1672-352x.20170524.003
投稿时间:2016-09-18
基金项目:2014校学科骨干培育项目(2014XKPY-65)资助。
Simultaneous determination of four arsenic species in chicken using liquid chromatography-hydride generation atomic fluorescence spectrometry
CHEN Dingding,GE Gaofei
(Biotechonlgy Center, Anhui Agricultural University, Hefei 230036)
Abstract:
An analytical method was developed for the simultaneous determination of four arsenic species including arsenite (As (Ⅲ)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), and arsenate (As(Ⅴ)) in chickens by liquid chromatography-hydride generation-atomic fluorescence spectrometry (HPLC-HG-AFS). The extraction of arsenic species from chicken samples was accomplished in 0.15 mol·L-1 nitric acid with ultrasonic wave. The different arsenic species were separated on a PRP-X100 anion exchange column and analyzed by HG-AFS. The mobile phase was 5 mmol·L-1 Na2HPO4 and 45 mmol·L-1 KH2PO4 buffer (pH5.92). The separation of four arsenic species were achieved in 8 min. A good linearity was obtained for all four arsenic species, with linear correlation coefficients being greater than 0.999. The detection limit(LODs)of the four species were between 1.0 and 3.0 μg·L-1. The relative standard deviations(RSD)in six replicated measures(100 μg·L-1)varied from 2.0% to 6.2%. The recovery rate for spiked chicken samples ranged from 82.1% to 101%.The method is simple and sensitive with a low operation cost and environmental friendly.
Key words:  arsenic species  liquid chromatography  hydride generation atomic fluorescence spectrometry  chicken

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