反相萃取结合GC-NCI-MS法测定水产品中甲基汞的含量

论文编号:SP092  论文字数:9213,页数: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

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