| Summary: | 碩士 === 國立高雄海洋科技大學 === 海洋環境工程研究所 === 102 === In the past, high performance liquid chromatography (HPLC) was used with the general total porosity column and the chromatography analysis duration cost a lot of time. Fortunately, the chromatography column with core particles has been developed in recent years. Its chromatography particles, sub-2.0μm, are with smaller diameter and better evenness compared with those in the general total porosity column. And among its filler particles, there is a solid silicon particle which makes the outer film thinner and the substance examined be able to balance fast between the stationary and the mobile phases, improving the separation efficiency of the chromatography.
Ascentis Express C18, a chromatography column with filler core particles, was applied in this study. Its length was 100 mm, inner diameter 4.6 mm and particle diameter 2.7 μm. The optimal conditions for the chromatography column with core particles found in this study included that the flow speed of the mobile phase was 1.0 mL/min, the mobile phase was acetonitrile: pH 4.0 H2O, and the percentages of the gradiently eluted acetonitrile were 12~20% (0~6 mins), 20~23% (6~10 mins) and 23% (10~15 mins), respectively. Eight sulfonamides were separated successfully.
Compared with general total porosity columns, the analysis duration each time cost fifteen minutes, saving 60% of analysis time. And, with the same concentration, the sensibility and resolution of the instrument increased significantly. Also, the signal width decreased significantly. On the other hand, the consumption of the organic solution, acetonitrile, reduced to 19 mL, saving 70% of acetonitrile. The instrument detection limit of HPLC/PDA fell from 2.0~120 to 1.9~6.0 μg/L. The instrument linear range was 20~5000 μg/L. The R square (r2) was over 0.999. The qualitative and quantitative precision, and the relative standard difference (n=7) of the retention time were below 0.2%. The relative standard difference of the peak area was 2.1~3.9% (n=7). Moreover, the height of theoretical plate (H) of the chromatography column with core particles was one tenth of that of the general total porosity column. The length of the chromatography column with core particles not only was shorter but also was with a larger number of theoretical plates (N).
The analysis method set up was applied to the analysis of the water samples from the ten inspection stations for the lakes and ponds that regulated the water volume in Tainan. The eight sulfonamides were not found (ND) in the water samples of Datan Pond and Daoye Lake, but all of them were found in the water samples of Yinghsi Lake. Among the eight sulfonamides, SMR was the most frequently detected and SMX and SMR were detected with the highest concentration due to that the main industries of Tainan were agriculture and livestock. Although the SMX concentration (0.69 μg/L) detected in the water samples was much lower than the median lethal concentration (18.3 μg/L) of SMX to plants as denoted in the literature, it was reported in a few literatures that the sulfonamides in the environment (water bodies) would increase the drug resistance of the organisms. Therefore, it is necessary to inspect the sulfonamides.
|
|---|
