碩士 / 國立中山大學 / 化學系研究所 / 104 / We have presented our research results in two parts, a first parts of research which is explained by, based on HPLC-ICP-MS for the simultaneous determination of Methyl-Hg, Hg(II) and Ethyl-Hg in fish oils. The separation was performed using ion-pair reversed-phase liquid chromatography on a C8 column with 0.6% (v/v) 2-mercaptoethanol, and 2.5% (v/v) MeOH as mobile phase using an isocratic elution. Separation of the three mercury species was carried out in less than 6.5 min. The detection limits for Methyl-Hg, Hg(II) and Ethyl-Hg were found to be 0.013, 0.014 and 0.026 ng mL-1, respectively. Reproducibility was less than 2% RSD for 5 replicate injections. Mercury species were extracted from fish oils by using an extractant, containing 0.6% (v/v) 2-mercaptoethanol, 2.5% (v/v) MeOH, 1% (m/v) lipase, 2% (m/v) Triton X-100, and 1.0% (v/v) nitric acid were also used to microwave assisted extraction procedure. The extraction efficiency of mercury achieved more than 90% at 60 oC within 5 min. The research results reveal that different mercury species were presented which depends on different brands of fish oil. However, Methyl-Hg and Hg(II) species were found in fish oil samples. Despite the fact that, there was no regulation about mercury for fish oils so far, the concentration of mercury was quiet low as compared to fish standards.
Second parts of results fully demonstrate based on HPLC-CV-ICP-MS for the simultaneous determination of Methyl-Hg and Hg(II) in edible mushroom samples. The vapor generation techniques were hyphenated liquid chromatography to enhance the sensitivity of mercury species. The separation was performed on C8 column with 0.6% (v/v) 2-mercaptoethanol, and 6.0% (v/v) MeOH as mobile phase, the separation of the mercury species was carried out in less than 6 min. The detection limits were also optimized, in Methyl-Hg and Hg(II) were found to be 0.011, and 0.029 ng mL-1, respectively. Reproducibility was less than 3.5% RSD for 5 replicate injections. Mercury species were extracted from mushroom samples using mobile phase as an extractant, containing 0.6% (v/v) 2-mercaptoethanol, and 6.0% (v/v) MeOH. The accuracy of the method was validated by using NRCC DOLT-3 Fish Liver Certified Reference. The Methodology were developed and applied to investigate mercury speciation in edible mushroom samples and results reveals that, which is predominantly presented in Hg(II) species. The concentration of Methyl-Hg was extremely low compared with Hg(II) concentrations. Finally, The developed method were optimized and applied to investigate mercury speciation in fish oils and mushroom samples.
| Identifer | oai:union.ndltd.org:TW/104NSYS5065084 |
| Date | January 2016 |
| Creators | Cheng-hung Yao, 姚承宏 |
| Contributors | Shiuh-jen Jiang, 江旭禎 |
| Source Sets | National Digital Library of Theses and Dissertations in Taiwan |
| Language | zh-TW |
| Detected Language | English |
| Type | 學位論文 ; thesis |
| Format | 101 |
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