摘要
建立了海产品中5种形态砷(As)的高效液相色谱-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V(甲醇)∶V(水)=3∶1溶液,70℃水浴振摇30 min提取1次,再用V(甲醇)∶V(水)=1∶1溶液提取2次,提取液用阴离子交换柱分离,以20 mmol.L-1碳酸铵[碳酸氢铵(NH4HCO3)+氨基甲酸铵(NH2COONH4)]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-1。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。
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.
出处
《南方水产科学》
CAS
CSCD
北大核心
2013年第2期50-56,共7页
South China Fisheries Science
基金
农业部引进国际先进农业科学技术计划重点项目“农产品中重金属形态分析技术引进与建立”(2010-G1-6)
关键词
海产品
砷形态
高效液相色谱
电感耦合等离子体质谱
测定
seafood
arsenic species
high performance liquid chromatography
inductively coupled plasma mass spectrometry
de-termination