【摘要】 以聚噻吩为萃取材料,优化对四环素类(TCs)抗生素的萃取条件,建立固相萃取-分光光度法(SPE-UV)、固相萃取-高效液相色谱法(SPE-HPLC)检测水体中TCs(OTC、TC、DOX)的分析方法。100 mL水样,调整pH=5.0,经50 mg聚噻吩萃取柱富集净化,甲醇/乙酸(V∶V=9∶1)解吸。SPE-UV法总量测定线性范围为0.15～2.4 mg/L,相关系数大于0.99;相对标准偏差为1.1%～4.5%(n=5);检出限为0.002 mg/L;对于100 mL 0.10 mg/L的TC和总量0.30 mg/L TCs标准溶液,萃取率分别为85%和70%;实际水样加标回收率99.7%～104%。SPE-HPLC法线性范围为0.005～1 mg/L,相关系数大于0.99;相对标准偏差为1.8%～3.0%(n=5);检出限为0.000 1～0.000 5 mg/L;对于100 mL0.010 mg/L的OTC、TC、DOX标准溶液,萃取率分别为74%、94%、58%;实际水样加标回收率98.8%～115%。应用两种方法对三种水样进行检测,仅由SPE-HPLC检出鱼塘水中含TC 1.0μg/L。更多还原

【Abstract】 Using polythiophenes as the extraction material and optimizing extraction conditions for tetracyclines(TCs), a solid phase extraction-spectrophotometric(SPE-UV) method and a solid phase extractionhigh performance liquid chromatography(SPE-HPLC) method were developed for the determination of TCs(OTC, TC, DOX) in water. The 100 mL water samples, adjusting the acidity to pH=5.0, were enriched and purified by 50 mg polythiophenes column and desorbed by methanol/acetic acid(V:V=9:1). SPE-UV method was used to measure the total TCs with linear range of 0.15-2.4 mg/L. The correlation coefficient was not less than 0.99.The relative standard deviationwas 1.1%-4.5%(n=5). The detection limits was 0.002 mg/L. For 100 mL of 0.10 mg/L TC and 0.30 mg/L total TCs standard solution, the extraction rates were 85% and 70%,respectively. The recoveries of standard in actual water were 99.7%-104%. The linear range of SPE-HPLC were 0.005-1 mg/L with the correlation coefficient not less than 0.99. The relative standard deviation were1.8%-3.0%(n=5). The detection limit were 0.000 1-0.000 5 mg/L. For 100 mL of 0.010 mg/L OTC, TC, DOX standard solution, the extraction rates were 74%, 94% and 58%, respectively. The recoveries of standard in actual water were 98.8%-115%. Three kinds of water samples were tested by two methods, and only TC was determined by SPE-HPLC in fish pond water with concentrations of 1.0 μg/L.更多还原