碩士 / 國立高雄海洋科技大學 / 海洋環境工程研究所 / 98 / Abstract
Although the government stipulates maximum residue level for the sulfonamides contained in animal medicine, sulfonamide abuse still exists in Taiwan. The ways approved by Taiwan government to test sulfonamides are with the shortcomings such as complicated procedure and time- and solvent-consuming. For those reasons, the improvement of the test methods is worth further study.
In this study, Taguchi L27orthogonal array experimental design was applied to discuss the microwave assisted extraction of the eight sulfonamides in fish. The purposes of the experiment were to: (1) explore whether there existed significant difference of the cross action between factor and factor; (2) seek for the optimization of the eight sulfonamides that were extracted in fish through microwave assisted extraction; (3) compare Taguchi L27 orthogonal array experimental design and the single factor method; (4) seek for the steadiness of the microwave assisted extraction in drawing out the eight sulfonamides in fish; (5) investigate the method detection limit of the microwave assisted extraction in drawing out the eight sulfonamides in fish; (6) compare microwave assisted extraction and method CNS14459; (7) set up the standard operation procedures for microwave assisted extraction in drawing out the eight sulfonamides in fish.
The result of the analysis of variance (ANOVA) showed that there was significant factor difference with respect to extraction solvent, extraction time and extraction temperature. It indicated that the level change inside the factor would affect the efficiency of the microwave assisted extraction in drawing out the sulfonamides in fish. As to the cross action between factor and factor, the cross action between extraction time and extraction solvent was with significant difference, which implied the change of extraction time and the necessity of the correct selection of solvents, which would affect the efficiency of the microwave assisted extraction in drawing out the sulfonamides in fish.
With average recovery 85~115% and relative standard deviation below 5%, after finishing 27 experiments, the following four optimizations were selected: (1) extraction with 20mL of acetonitrile at 100℃for 17.5 minutes; (2) extraction with 30mL of acetonitrile at 50℃ for 17.5 minutes;(3) extraction with 10mL of methanol at 50℃ for 17.5 minutes; 3) extraction with 20mL of methanol at 50℃ for 5 minutes. And those four optimizations met the ANOVA result already that the extraction solvent, extraction temperature and extraction time, and the cross action between extraction solvent and extraction time were with significant difference. And those four optimizations avoided that the optimization was estimated incorrectly due to that the single factor method neglected the cross action between factor and factor.
Regarding the method steadiness test, the intra-day and inter-day average recovery was 88.5%~103.6% and 85.0%~99.8%, respectively, and the intra-day and inter-day relative standard deviation was 0.3%~2.0% and 1.8%~8.8%, respectively. It was indicated that the accuracy was 85%~100% and the precision was below 10% pertaining to the steadiness of this method. And the method detection limit was 0.040μg/g~0.079μg/g, which was below the maximum residue level, 0.1μg/g, stipulated by Taiwan and the European Unit respectively. Consequently, it was inferred that the method was applicable to the test of the sulfonamides contained in fish.
In addition to, through the result of ANOVA, determining the significant difference between factor and factor and avoiding to neglect the optimization, this study method was with the advantages compared with method CNS14459, including simple procedures (one extraction one purification), time saving (two hours), solvent saving (20 mL), excellent method steadiness (both all the intra-day and inter-day accuracies were 85~100% and all the precisions were below 10%), low method detection limit (0.040μg/g~0.079μg/g, below the stipulation required maximum residue level).Therefore, it was concluded that the method was applicable to the test of the eight sulfonamides contained in fish.
| Identifer | oai:union.ndltd.org:TW/098NKIM8282001 |
| Date | January 2010 |
| Creators | wu,cheng-lin, 吳政霖 |
| Contributors | 陳秋雲 |
| Source Sets | National Digital Library of Theses and Dissertations in Taiwan |
| Language | zh-TW |
| Detected Language | English |
| Type | 學位論文 ; thesis |
| Format | 95 |
Page generated in 0.0014 seconds