液相色谱-氢化物发生-原子荧光光谱法测定干制食用菌中5种砷形态

Determination of 5 kinds of arsenic species in dried edible mushrooms by liquid chromatography-hydride generation-atomic fluorescence spectrometry

中文关键词:  干制食用菌  砷形态  液相色谱-氢化物发生-原子荧光光谱法

英文关键词:dried edible mushroom  arsenic species  liquid chromatography-hydride generation-atomic fluorescence spectrometry

中文摘要:

      目的 建立液相色谱-氢化物发生-原子荧光光谱法(liquid chromatography-hydride generation-atomic fluorescence spectrometry, LC-HG-AFS)同时测定干制食用菌中砷甜菜碱(arsenobetaine, AsB)、砷酸根[arsenate, As (Ⅴ)]、亚砷酸根[arsenite, As (III)]、一甲基砷(monomethylarsonic acid, MMA)和二甲基砷(dimethylarsenic acid, DMA)的方法。方法 样品用水于60 ℃水浴超声提取1.5 h, 离心10 min取上清液, 经0.45 m滤膜过滤。采用Hamilton PRP-X100阴离子交换柱(250 mm×4.1 mm, 10 μm), 以8 mmol/L磷酸氢二铵(pH 8.5)为流动相进行分离, 用LC-HG-AFS法测定5种砷形态。结果 AsB、MMA、DMA和As (III)在2.5~200.0 μg/L范围内线性关系良好, As (Ⅴ)在5.0~200.0 μg/L范围内线性关系良好, 5种砷形态标准曲线相关系数均大于0.999; 5种砷形态加标回收率为85.0%~107.0%, 相对标准偏差均小于5.0%; AsB、MMA、DMA、As (III)和As (Ⅴ)的检出限分别为0.02、0.02、0.01、0.02和0.03 mg/kg, 定量限分别为0.04、0.04、0.03、0.06和0.08 mg/kg。结论 所建方法简便、准确、快速, 适用于干制食用菌中AsB、MMA、DMA、As (III)和As (Ⅴ)的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of arsenobetaine (AsB), arsenate [As (Ⅴ)], arsenite [As (III)], monomethylarsonic acid (MMA) and dimethylarsenic acid (DMA) in dried edible mushrooms by liquid chromatography-hydride generation-atomic fluorescence spectrometry (LC-HG-AFS). Methods The samples were ultrasonically extracted with water in water bath at 60 ℃ for 1.5 h, centrifuged for 10 min, and the supernatants were filtered by 0.45 m microporous membrane and separated on a Hamilton PRP-X100 anion exchange column (250 mm×4.1 mm, 10 m) using 8 mmol/L diammonium hydrogen phosphate (the pH was 8.5) as mobile phase. The 5 kinds of arsenic species were determined by LC-HG-AFS. Results AsB, MMA, DMA and As (III) had a good linear relationship in the range of 2.5–200.0 μg/L, and As (V) had a good linear relationship in the range of 5.0–200.0 μg/L, and the standard curve correlation coefficients of 5 kinds of arsenic species were all greater than 0.999. The spiked recoveries of 5 kinds of arsenic species were 85.0%–107.0%, and relative standard deviations were all less than 5.0%. The limits of detection of AsB, MMA, DMA, As (III) and As (Ⅴ) were 0.02, 0.02, 0.01, 0.02 and 0.03 mg/kg, respectively, and the limits of quantitation were 0.04, 0.04, 0.03, 0.06 and 0.08 mg/kg, respectively. Conclusion This method is simple, accurate and rapid, and suitable for the determination of AsB, MMA, DMA, As (III) and As (Ⅴ) in dried edible mushrooms.