作者：王怡梅, 江维, 李漂洋, 胡晓荣

作者单位：成都理工大学材料与化学化工学院，四川 成都 610059

关键词：聚噻吩;四环素类;固相萃取;养殖水

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0.0001~0.0005 mg/L；对于100 mL 0.010 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 1.0 μg/L。

Determination of tetracyclines in water using polythiophenes extraction and UV&HPLC
WANG Yimei, JIANG Wei, LI Piaoyang, HU Xiaorong
College of Materials and Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China
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 extraction-high 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 were 1.8%-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.

Keywords: polythiophenes;tetracyclines;solid phase extraction;aquaculture water
2020, 46(8):63-69  收稿日期: 2020-06-30;收到修改稿日期: 2020-07-25
基金项目:
作者简介: 王怡梅（1995-），女，四川资阳市人，硕士研究生，专业方向为分析化学
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