| 熊文明，冯敏铃，李拥军，李男，李盛安，招钰娟，林庆昶.微波辅助提取-高效液相色谱-电感耦合等离子体质谱法测定水产品中甲基汞和乙基汞[J].广东农业科学,2013,40(13):101-103 |
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微波辅助提取-高效液相色谱-电感耦合等离子体质谱法测定水产品中甲基汞和乙基汞 |
| Determination of methylmercury and ethylmercury in aquatic products by microwave -assisted extraction coupled with high performance liquid chromatography-inductively coupled plamas mass spectrometry |
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| DOI： |
| 中文关键词: 微波辅助提取 高效液相色谱-电感耦合等离子体质谱法 水产品 甲基汞 乙基汞 |
| 英文关键词: microwave-assisted extraction high performance liquid chromatography-inductively coupled plamas mass spectrometry (HPLC-ICP/MS) aquatic products methylmercury ethylmercury |
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| 摘要点击次数: 1457 |
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| 中文摘要: |
| 建立了水产品中甲基汞和乙基汞的微波辅助提取-高效液相色谱-电感耦合等离子体质谱（HPLC-ICP -MS）测定方法。为保证样品中汞的各形态能完全提取并准确分析，通过条件优化，使用5 mol/L盐酸溶液微波辅助提取样品中的甲基汞和乙基汞，流动相为0.01 mol/L乙酸氨、0.12%(V/V) L-半胱氨酸、8% (V/V) 甲醇-水溶液。提取液在液相色谱中分离后，进入电感耦合等离子体质谱检测，5 min内完成甲基汞和乙基汞的定量分析。在优化的检测条件下，甲基汞和乙基汞检出限分别可达到0.024、0.042 μg/L吗，在0.05~20 μg/L范围内均具有良好的线性关系，相关系数均为0.9999，平均加标回收率为84.0%~94.5%。两种汞形态的批内和批间相对标准偏差分别在2.1%~4.1%和2.6%~4.3%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，满足汞形态定量分析的要求。 |
| 英文摘要: |
| A high performance microwave-assisted extraction-high performance liquid chromatography-inductively coupled plamas mass spectrometry （HPLC-ICP/MS）method was developed for determination of methylmercury and ethylmercury in aquatic products. In this experiment, methylmercury and ethylmercury were extract from the aquatic products with microwave assisted, and 5 mol/L hydrochloric acid solution used as extraction solvent. 8% (V/V) methanol aqueous solution containing 0.12% (V/V) L- cysteine and 0.01mol/L ammonium acetate buffer were used as mobile phase. The quantitative analysis of target compounds was carried out by HPLC-ICP/ MS within 5 minutes. Under the optimized conditions, the detection limit of methylmercury and ethylmercury were up to 0.024 μg/L and 0.042 μg/L, there were good linear relationships in the 0.05~20 μg/L for methylmercury and ethylmercury, and the correlation coefficients were 0.9999. The average spiked recoveries ranged from 84.0% to 94.5%. The relative standard deviations of intra-batch and inter-batch were in the range of 2.1%~4.1% and 2.6%~4.3%, respectively. This method was simple, rapid, sensetive and accutate, meet the mercury speciation quantitative requirements. |
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