高效液相色谱一电感耦合等离子体质谱联用技术测定海产品中5种形态砷

建立了海产品中5种形态砷（As）的高效液相色谱一电感耦合等离子体质谱联用测定方法。将样品冷冻干燥后采用矿（甲醇）：V（水）=3：1溶液，70℃水浴振摇30rain提取1次，再用y（甲醇）：y（水）=1：1溶液提取2次，提取液用阴离子交换柱分离，以20mmol·L-1碳酸铵碳酸氢铵（NH。HCO，）＋氨基甲酸铵（NH：COONH。）]为流动相，用电感耦合等离子体质谱检测。5种As的检出限为0．057～0．13μg·L-1，定量限为0．19～0．43μg·kg。添加回收率为83．2％～115％，相对标准偏差小于10％。实际海产品样品测定结果表明，海产品中的As主要以砷甜菜碱和二甲基砷酸为主，5种形态As的和与总As相比，总体提取率达90％以上。

Determination of five arsenic species in seafood using high performance liquid chromatography (HPLC) coupled with inductively coupled plasma mass spectrometry (ICP-MS)

A method was established to determine five arsenic species in seafood using high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry （HPLC-ICP-MS）. Freeze dried samples were extracted with methanol-water （3：1 ） shaking in 70 ~C water bath for the first time, and extracted with methanol-water（ 1：1 ） for the second and third time. Then we separa- ted the extract by anion exchange column using 20 mmol-L- 1 NH4 HCO3 ＋ NH2 COONH4 mobile phase, and detected the compounds with plasma mass spectrometry. The detection limit and quantification limit of five arsenic speciations in seafood varied from 0. 057 - 0. 13 pog.L-land from 0. 19 ~0. 43 p.g,kg ~. The average recovery of five species arsenic spiked in tested samples at 3 levels ranged from 83.2% - 115% with the relative standard deviation （RSD） between 2.15% and 9.97%. The proposed method had been applied to the analysis of seafood came from Australia, indicating that arsenobetaine （AsB） and dimethylarsinic acid （DMA） were main spe- cies of arsenic in seafood, and the extraction efficiency of five arsenic speciations were more than 90% , which was higher than of total arsenic.