你好,欢迎来到经管之家 [登录] [注册]

设为首页 | 经管之家首页 | 收藏本站

反相萃取结合GC-NCI-MS法测定水产品中甲基汞的含量_食品科学与工程论文

发布时间:2015-04-01 来源:人大经济论坛
食品科学与工程论文范文 目 录 中文摘要I 英文摘要II 目录III 1. 绪论1 1.1汞的主要来源1 1.1.1自然界中的汞1 1.1.2工业来源1 1.1.3垃圾中的汞排放1 1.1.4 电子产品中的汞2 1.2汞的主要用途2 1.3汞的存在形式3 1.4甲基汞的毒害作用3 1.4.1甲基汞在食品中的危害3 1.4.2甲基汞在环境中的危害4 1.5甲基汞的作用机理4 1.6甲基汞的检测方法4 1.6.1苯萃取法5 1.6.2巯基棉富集法5 1.6.3固相萃取法5 1.6.4蒸馏法5 2. 实验部分6 2.1原理6 2.2材料与方法6 2.2.1材料6 2.2.2试剂配制6 2.2.3标准物质的配制6 2.2.4质谱条件6 2.2.5仪器7 2.3方法7 2.3.1实验操作步骤7 2.3.2实验条件讨论7 2.3.3标准曲线的绘制及相关系数实验9 2.3.4样品加标回收率的实验9 2.3.5样品的检测实验10 3. 结果与讨论11 3.1方法的线性11 3.1.1标准曲线和相关系数11 3.1.2样品加标回收率,精密度和检出限11 3.1.3方法检出限和检测限11 3.1.4样品的检测实验结果13 3.2反相萃取法与其他前处理方法的比较13 4.总结与展望15 4.1反相萃取-气质联用法测定水产品中甲基汞含量方法的建立15 4.2反相萃取法测定水产品中甲基汞含量测定的注意事项15 4.3该方法存在的问题以及今后的研究方向16 致谢17 参考文献18 摘要:甲基汞(CH3Hg)是蓄积性重金属污染物汞的主要存在形式,是一种剧毒性物质,它的毒性是其它汞化合物毒性的几百倍。它可以通过富集作用在体内积蓄,损害人的神经系统。水俉病即为甲基汞慢性中毒症。本实验以鳙鱼,青虾和梭子蟹为例来建立采用苯萃取和L-半胱氨酸滤纸富集再用苯洗脱,使甲基汞得到富集和净化,再用气质联用仪进行测定,初步建立了反相萃取结合GC-NCI-MS法测定水产品中甲基汞含量的方法。还运用此方法检测梭子蟹、小龙虾等十种水产品中甲基汞的含量。样品经过苯萃取之后,经HP-5MS色谱柱分离,SIM离子检测器检测,以保留时间和质荷比定性,峰面积定量,研究表明甲基汞标准溶液在0.1μg/mL~2μg/mL范围内有良好的线性关系,关系式为Y=124283.879X-1728.8744,相关系数为0.99911。样品的回收率在92%-103%之间,此方法准确度显著于常规的苯萃取方法,和巯基棉富集法相比可以避免乙酸酐和浓硫酸等易制毒化学品的使用。本方法准确可靠、操作简便、易于推广、灵敏度高、重现性好和检出限低等优点,能满足水产品中甲基汞残留量检测的要求。 关键词:反相萃取;GC-NCI-MS;水产品;甲基汞 Abstract:Methylmercury (CH3Hg) is the accumulation of heavy metals pollutants who is the main form of mercury. while is the toxicity of other toxic mercury compounds of several hundredfold. It can be enriched through the role of savings in the body and damage the nervous system. Wu is the water of methylmercury chronic poisoning disease. This experiments use bighead carp, Macrobrachium nipponense and blue crab as an example to the establishment of a benzene extraction and L-cysteine filter paper recycling benzene renounce and then GC-MS instrument Determination,and the initial establishment of the GC-NCI-MS. We also use this method to detect blue crab, crayfish and other aquatic products in the methylmercury content. After samples of benzene extraction, the HP-5MS column separation, SIM-detector test, to preserve the time and quality than could be qualitative, quantitative peak area, the study showed that methylmercury standard solution in the 0.1 μg/mL -2.0 μg/mL within the framework of a good linear relationship, the relationship between the Y=124283.879X-1728.8744, a correlation coefficient of 0.99911. Samples of the recovery of between 92% -103%, this method significantly the accuracy of the benzene in the conventional extraction methods, and sulfhydryl enrichment of cotton compared to avoid sulphuric acid and acetic anhydride, and aslo precursor chemicals in use. This method is accurate and reliable, simple, easy to promote, sensitive, reproducible and low detection limits and strengths to meet the methyl mercury residues in aquatic products in the testing requirements. Key words: RP-extraction; GC-NCI-MS; aquatic products; methylmercury
经管之家“学道会”小程序
  • 扫码加入“考研学习笔记群”
推荐阅读
经济学相关文章
标签云
经管之家精彩文章推荐