色谱2011，Vol.29Issue(7)：667-672,6.DOI:10.3724/SP.J.1123.2011.00667
水产品中甲基汞测定的液相色谱-原子荧光光谱联用方法的改进
Improvement of the method for methylmercury determination in aquatic products using liquid chromatography online coupled with atomic fluorescence spectrometry
摘要
Abstract
The improvement method was developed for methylmercury determination using liquid chromatography online coupled with cold vapor atomic fluorescence spectrometry ( LC-CVAFS ). Cysteine was used as complexing agent in mobile phase instead of mercaptoethanol.Under the optimized conditions , baseline separation of mercury species could be achieved within 8 min on a C18 column with a mobile phase of 5％ ( V/V ) acetonitrile-1 g/L L-cysteine-50 mmol/L ammonium acetate aqueous solution. The linear range of calibration curve of methyl-mercury was 1 - 50 μg/L and the limit of detection ( S/N = 3 ) for methylmercury was 0.3 μg/L.Ultrasonication assisted hydrochloric acid extraction was used to extract methylmercury from seafood samples. The sample extract was cleaned up by a C18 solid phase extraction ( SPE )cartridge. For validation of the method, certified reference materials and spiked seafood samples were analyzed. The determined methylmercury contents of certified reference materials NIST1566b、BCR464 and GBW10029 agreed well with the certified values. The determined methylmercury values for Food Analysis Performance Assessment Scheme ( FAPAS ) sample 07115 were satisfied. The recoveries of methylmercury in seafood samples at three spiked levels ( 10,50 and 500 μg/kg ) ranged from 89％ to 112％ , including cooked seafood food. The precision of the method based on relative standard deviation ( RSD ) was not more than 7％. The present method of LC-CV-AFS is accurate, sensitive, simple, and can meet the demand of methylmer-cury determination in seafood.关键词
液相色谱/原子荧光光谱/甲基汞/形态分析/水产品Key words
liquid chromatography ( LC )/ atomic fluorescence spectrometry( AFS )/ methyl-mercury / species analysis / aquatic products分类
化学化工引用本文复制引用
尚晓虹,赵云峰,张磊,李筱薇,吴永宁..水产品中甲基汞测定的液相色谱-原子荧光光谱联用方法的改进[J].色谱,2011,29(7):667-672,6.基金项目
"十一五"国家科技支撑计划项目(2006BAK02A10)和卫生行业公益项目(200902009). （2006BAK02A10）
