Zhang Lei, Zhou Rui, Li Xiao-wei, Zhao Yun-feng, Liu Li-ping, Wu Yong-ning
National Institute for Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing, China.
Zhonghua Yu Fang Yi Xue Za Zhi. 2008 May;42(5):298-303.
To develop a method for determining arsenobetaine (AsB), arsenite (AsIII), arsenate (AsV), Monomethylarsonic acid (MMA) and Dimethylarsenic acid (DMA) with liquid chromatography (LC), on-line UV-decomposition (UV), hydride generation (HG) and atomic fluorescence spectrometry (AFS) in animal origin seafood samples.
Arsenic compounds were extracted in an ultrasonic bath with methanol-water (9:1) solvent from the animal origin seafood samples. The extracts were evaporated with N2 and dissolved in water. The solvent was extracted by hexane to remove lipids. And then, the aqueous solution was diluted to 10 ml. The extracts were filtered before analysis by LC-AFS. The mobile phase consisted of 0.5 mmol/L NH4H2PO4 (pH 9.0) and 20 mmol/L NH4H2PO4 (pH 6.0). Arsenic species were separated with an anion exchange column Hamilton PRPX-100 and gradient elution, detected by LC-UV-HG-AFS.
The established separation condition could achieve a better separation for five arsenic species. Detection Limits (LOD) were ranged from 0.0025 to 0.0032 mg/L, AsB was the predominant arsenic species in the animal origin seafood samples. AsIII and DMA were detected in certain shellfish samples at trace level. The accuracy of total arsenic measurement was tested by the analysis of NBS 1566 (Oyster Tissue). The accuracy of arsenic species measurement was tested by the analysis of BCR 627 (Tuna Fish). The data were tallied with the certified value.
Arsenic species were specifically detected by LC-UV-HG-AFS in the animal origin seafood samples.
建立一种采用液相色谱（LC）、在线紫外消解（UV）、氢化物发生（HG）和原子荧光光谱法（AFS）测定动物源海鲜样品中砷甜菜碱（AsB）、亚砷酸盐（AsIII）、砷酸盐（AsV）、一甲基胂酸（MMA）和二甲基胂酸（DMA）的方法。
用甲醇 - 水（9:1）溶剂在超声浴中从动物源海鲜样品中提取砷化合物。提取物用氮气蒸发并用水溶解。用己烷萃取溶剂以去除脂质。然后，将水溶液稀释至10 ml。提取物在通过LC - AFS分析之前进行过滤。流动相由0.5 mmol/L NH4H2PO4（pH 9.0）和20 mmol/L NH4H2PO4（pH 6.0）组成。砷形态用阴离子交换柱Hamilton PRPX - 100进行分离并梯度洗脱，通过LC - UV - HG - AFS进行检测。
所建立的分离条件能够对五种砷形态实现较好的分离。检测限（LOD）在0.0025至0.0032 mg/L之间，AsB是动物源海鲜样品中的主要砷形态。在某些贝类样品中检测到痕量水平的AsIII和DMA。通过分析NBS 1566（牡蛎组织）测试总砷测量的准确性。通过分析BCR 627（金枪鱼）测试砷形态测量的准确性。数据与认证值相符。
通过LC - UV - HG - AFS在动物源海鲜样品中特异性检测到砷形态。
Zotero 插件