| 熊文明，冯敏玲，李拥军，李男，李盛安，招钰娟，林庆昶.超声辅助提取-高效液相色谱-电感耦合等离子体质谱法测定南美白对虾中砷形态[J].广东农业科学,2013,40(12):122-124 |
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超声辅助提取-高效液相色谱-电感耦合等离子体质谱法测定南美白对虾中砷形态 |
| Determination of Arsenic speciation in Penaeus vannmei by ultrasonic-assisted extraction-HPLC-ICP/MS |
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| DOI： |
| 中文关键词: 超声辅助提取 高效液相色谱-电感耦合等离子体质谱法 南美白对虾 砷形态 |
| 英文关键词: ultrasonic-assisted extraction HPLC-ICP/MS Penaeus vannmei Arsenic speciation |
| 基金项目:中山市科技计划项目（20114A195） |
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| 中文摘要: |
| 应用超声辅助提取-高效液相色谱-电感耦合等离子体质谱法（HPLC-ICP/MS）测定南美白对虾中的砷形态。以磷酸-水（1：19，V/V）混合液作为萃取剂，超声辅助提取样品中的砷化合物，采用Hamiton PRP-X100柱分离砷化合物，以20mmol/L磷酸氢二铵溶液（pH=9.0）为流动相。在优化的检测条件下，9min内完成4种砷化合物的定量分析，亚砷酸尧砷酸、MMA（V）和砷甜菜碱检出限分别可达到0.3、0.7、0.6、0.8μg/L，在2.5~100μg/L范围内均具有良好的线性关系，相关系数均在0.995以上，平均加标回收率为82.5%~98.0%，4种砷形态的批内和批间相对标准偏差分别在2.9%~4.9%和3.1%~4.8%的范围内。该方法具有简单、快速、灵敏度高和定性准确等优点，满足砷形态定量分析的要求。 |
| 英文摘要: |
| The speciation of arsenic in Penaeus vannmei was analyzed using microwave-assisted extraction-high performance liquid chromatography-inductively coupled plamas mass spectrometry（HPLC-ICP/MS）method. arsenic compound were extracted from the aquatic products with microwave assisted, and 50%(V/V) methanol aqueous solution was used as extraction solvent. The column of Hamiton PRP-X100 was used to separate the arsenic species, and 20 mmol/L ammonium dihydrogen phosphate solution with the pH adjusted to 9.0 was used as mobile phase. The quantitative analysis of target compounds was carried out by HPLC-ICP/MS within 9 min.Under the optimized conditions, the detection limit of arsenious acid, arsenic acid, MMA(Ⅴ) and AsB were up to 0.3,0.7,0.6,0.8μg/L,respectively. There were good linear relationships in 2.5~100μg/L for four arsenic compounds, and the correlation coefficients were up to 0.995. The average spiked recoveries ranged from 82.5% to 98.0%. The relative standard deviations of intra-batch and inter-batch were in the range of 2.9%~4.9% and 3.1%~4.8%, respectively. This method was simple, rapid, sensetive and accutate, met the arsenic speciation quantitative requirements. |
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