摘要
建立了采用超声辅助提取,高效液相色谱-电感耦合等离子体质谱联用技术测定水产及其制品中汞形态分析的方法。在盐酸+L-半胱氨酸体系下,对样品进行超声辅助萃取,以10mmol/L乙酸铵+0.10%L-半胱氨酸缓冲盐与甲醇(体积比982)组成流动相,用高效液相色谱-电感耦合等离子体质谱仪同时检测无机汞、甲基汞和乙基汞的含量。无机汞、甲基汞和乙基汞的检出限(3S/N)分别为0.18,0.09,0.15ng/mL,标准曲线回归方程相关系数(R)均>0.999。以实际样品对无机汞、甲基汞、乙基汞进行加标回收试验,回收率在78.5%~96.8%,相对标准偏差(RSD)≤3.0%。经对标准物质进行检测,测得值与标准值吻合。该方法准确可靠、简单快速、精密度及准确度结果理想,可用于实际水产及其制品中汞形态的分析。
Ultrasonic assisted extraction coupled with high performance liquid chromatography-inductively coupled plasma mass spectrometry was developed for the determination of mercury speciation in aquatic products.Using ultrasonic assisted extraction for sample in HCl＋ L-cysteine system,with 10mmol/L ammonium acetate＋0.10% L-cysteine buffer and methanol（982）system consisting of mobile phase,and detected the content of inorganic mercury and methyl mercury and ethyl mercury by high performance liquid chromatography-inductively coupled plasma mass spectrometry.The detection limits（3S/N）of inorganic mercury,methyl mercury and ethyl mercury were 0.18,0.09,0.15ng/mL,respectively.The correlation coefficient（R）of the regression equation of the standard curve was above 0.999.Inorganic mercury and methyl mercury,ethyl mercury were spiked in actual samples,the rate of recovery was 78.5%~96.8%,the relative standard deviation（RSD）≤3.0%.The standard substance was detected by this method,and the measured value was consistent with the standard value.The method is accurate,reliable,simple,rapid and accurate.It can be applied to the analysis of mercury speciation in aquatic products.
出处
《食品与机械》
CSCD
北大核心
2017年第7期65-69,154,共6页
Food and Machinery
基金
河南省科技厅科技攻关项目(编号:162102310065)
